09931145H Syngistix For ICP Software Guide
09931145H Syngistix For ICP Software Guide
Software Guide
Syngistix™ for ICP
Software Guide
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ii . Syngistix Software Guide
Release History
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User Assistance
PerkinElmer, Inc.
710 Bridgeport Avenue
Shelton, Connecticut 06484-4794
U.S.A.
Notices
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Syngistix is a trademark of PerkinElmer, Inc.
Table of Contents
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Related Applications
In addition to the Syngistix software, PerkinElmer provides:
• The Data Manager software application lets you archive, copy, backup, delete, and
rename the data sets created by Syngistix. Within this application, you can select a subset
of the data from a results data set and save it in a file format that can be read by many
off-the-shelf applications, including spreadsheet and database management programs. In
addition, you can create printed reports of data where you control the design of and the
information included in the report.
• The User Setup software application to set up and control Users & Groups, Data Folders,
Email Setup, Notifications, and Settings (for Application Lockout times). If you have the
Enhanced Security (ES) version, manage Electronic Signatures.
• Syngistix Offline is a second copy of the Syngistix application that does not control the
instrument. You can use Syngistix to edit methods, enter sample information, examine data,
build IEC or MSF models, or reprocess data in the software without operating the instrument.
This is useful when you wish to work with methods and data while an analysis is in progress.
• If you have the Enhanced Security (ES) version, the ES Tools application the provides you
with the ability to Review and Approve/Reject methods and samples.
Introduction to Syngistix . 3
I m portant Prerequisites
Before you use Syngistix software, you should:
• Understand ICP principles and practices. If you need background information,
you should consult one of the many textbooks available.
• Know how to use a personal computer. If you need further information, consult
your computer manual.
• Understand Windows fundamentals. If you have questions, refer to manuals,
books, USB stick, CD-ROM, or online tutorials on Microsoft Windows.
4 . Syngistix™ Software Guide
• A complete list of units that can be selected in the Syngistix software are contained
in a file called “units.inix” located in the directory:
C:\Users\Public\PerkinElmer Syngistix\ICP\SystemFiles\Configuration
Edit this file (using Notepad) to rearrange, delete, or add units. Instructions for
editing the file are contained in the file.
• You can save the layout of windows on the screen and the names of files currently
open by selecting Workspace from the Application button then use the Save As
command. To recall the workspace and arrange the screen as it was saved, use the
Workspace Open command.
• You can check a method for internal consistency by selecting the Check Method
command from the Method group on the Analysis tab. Any problems discovered will
be reported in a dialog. The same check is automatically performed when the
method is saved and before it is used to analyze samples.
• To print an analytical header during a manual analysis, select the Analytical Header
command from the Analysis menu.
• You can display information on the instrument hardware components attached to
your system by selecting the Diagnostics in the Utilities group, on the Instrument
tab. Each component has a page of information showing its status and commands
that have been exchanged between computer and hardware.
• The system "signs" the data for each sample when it is stored in the results library.
Use the Verify Data Set... command in the Data Manager to check that no changes
have been made since the data were collected by the instrument.
• Select Syngistix Offline from the Applications group on the Utilities tab to display a
second copy of the application where you can edit methods, enter sample
information, examine data, build IEC or MSF models, or reprocess data while
analyses are in progress.
• You can display the autosampler locations for all samples, blanks, standards, and
quality control samples in the currently selected methods and sample information file
using the Autosampler Loading List window.
• When performing multi-method analyses, use the Autosampler Loading List window
to display the ___location of all solutions required by all methods to be sure the
locations are compatible.
• You can automatically export your data as a tab or comma delimited ASCII file at the
end of analyses. Create the export design using the Data Manager, then select it
using the Automatic Export command in the Options menu.
• See the Syngistix Document Pack for application notes, technical papers, and
documents that describe specialized features of the system such as a description of
the file formats used by the software.
• You must analyze the calibration blank before the calibration standards if the
selected calibration algorithm requires a blank. If it is analyzed after the standards,
errors will result.
• You can temporarily delete one or more analytes in a method by selecting the
Enable/Disable Elements... command from the Analysis menu and choosing the
analytes to disable from the dialog that is displayed.
• Using the Scheduler, you can schedule the instrument to automatically shut itself
down at the conclusion of analyses and to automatically start-up again so that it is
ready to perform analyses when you arrive in the morning.
6 . Syngistix™ Software Guide
• The system automatically performs a series of checks when you begin analyses to
detect mistakes or conditions that must be corrected before analyses can proceed.
• If you have occasional samples with high concentrations of analyte, it is possible to
schedule an extra wash step following them to minimize carry over to the next
sample. Schedule the extra wash step on the Sampler page of the Method Editor.
• Reagent blanks can be used to compensate for contamination of the samples by the
reagents used during the sample preparation process. Reagent blanks are selected
and scheduled on the Calibration page of the Method Editor.
• If you are only interested in using a small part of the calibration range or if you
cannot prepare a valid calibration blank for some reason, use the bracketing
calibration curve equation options.
• Normally when a method is opened the calibration curves are cleared and new
calibration curves are prepared as the blanks and standards are analyzed. However,
it is possible to automatically load existing calibration curves along with the method
by making selections on the Calibration page of the Method Editor.
• Quality control samples can be automatically analyzed at periodic intervals. The QC
samples are defined on the QC page of the Method Editor. Scheduling can also be
defined as part of the method or, alternatively, as part of the sample information file.
• When one or more measured concentrations in a quality control sample is not within
predefined limits, the system will automatically perform appropriate actions such as
recalibration, recalibration and reanalyzing samples, printing messages, or stopping
the analyses.
• The amount of information to be printed on the log during analyses can be selected
on the Options page of the Method Editor.
• The individual raw spectra can be saved with the other analytical data in the results
library. Saving spectra allows the data to be examined and used to recalculate the
analytical results using different analytical parameters, but requires more disk space.
Turning off this option saves disk space.
• You can have the system play sounds at the end of long operations or if problems
develop during analyses. Choose the Notifications from the Applications button
to turn sounds on or off and to select .wav files containing the sounds you want to
hear.
• Use the Sample Information Editor to enter descriptive information about your
samples such as sample ID's (names), weight and dilution information, autosampler
locations, and descriptive remarks.
• The Wavelength Table window allows you to search a database containing about
50,000 wavelengths. The table also contains recommended lines for most elements
and performance information for many of the lines that can be measured using an ICP.
Introduction to Syngistix . 7
Ribbon Style Interface - Consolidates the Workflow to 4 tabs with no hidden menus.
Data Viewer - This is a tabular data view to compliment the classic results view.
Expandable Windows (specifically Continuous Graphics, as more time/data points are
added if you expand horizontally)
Updated graphics and user interfaces - Provides a clean look to view your data and
information.
Consolidated Analysis Window - Combines Automated and Manual analysis with a
common run list in one window.
Status Panel (with quick links) - Provides a quick view of your current status and by
double-clicking a graphic to display its associated dialog.
Right-click Menus for Display Options - Provides easy navigation to functions in dialogs.
Most Recently Used Mechanism - Displays the last five methods/files opened.
Combined Devices Window - Puts your devices in one dialog for easy control.
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Data M anager
The Data Manager is a Syngistix application that helps you organize and manage the data
stored in libraries. You can rename, copy, archive, and delete data sets.
Im portant Note: Library maintenance should be done periodically to prevent your Results Library
from becoming too large. A large Results Library can lead to disk problems.
Maintenance procedures include archiving, deleting, and packing data sets. For
additional information, please refer to Data Manager Help: What's Important
About Managing Data.
Files
Not all Syngistix information is stored in database libraries. For example, sample information
is stored in ASCII files, so that you can easily create compatible sample information files
using off-the-shelf applications such as spreadsheet programs. You can use the Windows
Explorer to copy, rename, move, or delete these files.
Different Libraries
You may want to create separate libraries for each person using the system. You can do this
by creating new libraries for the methods and results using Data Manager. Refer to the Data
Manager Help file for information.
Softw are Overview
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Application Button
Clicking on the Application button provides the following commands that are available at all
times:
W ork space
Workspace let you store a group of selected windows for later use. The workspace saves all of
the entries you have made in the windows for your methods and analyses. It also saves the
___location of each window on the screen. The workspace is saved in a workspace file, which has
the extension .ifsx. Using workspaces, you can fill in and arrange windows once, saving time
whenever you set up methods or perform analyses.
Entries that you can save using a workspace include the names of the method and sample
information file, information contained in the Automated Analysis window (Set Up page), and
any information concerning multi-method analysis. It also saves decisions that you have made
for your analysis, such as if data is to be saved and where, if it is to be printed, and if the
method in memory is to be used.
Note: When you close Syngistix, the current Workspace is automatically saved and will redisplay
when you restart Syngistix.
To create a workspace:
1. Open the desired windows, fill in the entries for your methods and analyses and arrange the
windows on the screen.
For example, suppose you have run an analysis and arranged the windows as follows:
2. You can save the entire screen with all of the displayed windows and entries in a
"Workspace" file to redisplay later.
3. To save the position of these windows and the entries within them, from the
Application button select Save As from the Workspace menu item.
4. In the dialog that appears, type a name for the workspace and click the Save button.
For example, suppose you type "analysis".
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5. When you wish to view (or use) these windows and their entries again, in the
Application button, select Workspace then Open.
6. In the dialog that appears, select a saved file and click on Open. The windows with the
entries appear exactly as before.
Notifications
Users may elect to play sounds (to notify them) at the end of certain tasks to signal completion
or to signal their attention. Sounds are included in the software and are located in the same
drive in which the application was installed. In order to use sounds, you must have a sound
card installed in your computer. In addition to a sound a user can get an Email or text
notification.
To display this dialog:
Note: You may use any Windows sound files with a .wav document extension or any .wav sound files
that you might have installed.
Sounds are set to defaults and are interchangeable. For example, you may replace the
End of Analysis sound with that of the QC Failure.
5. After you have checked the appropriate sounds and their related .wav files, click on OK.
The name of the .wav file displays in the Select Sound Effect column in the
Notifications dialog..
Note: Before setting email notifications in this dialog, set up the email in the User Setup application.
Refer to the instructions for Email Setup in the User Setup Software Guide (P/N 09931535) of
the User Setup help file.
4. Click OK.
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1. On the Instrument tab, in the Quick Start group, click on the Express Analysis
button.
The Quick Start dialog appears.
3. Optionally, if you desire, click the Select Workspace drop-down button v and select
Open or a Recent Workspace name from the drop-down list.
You don't need to select a Workspace to run Quick Start.
Note: Select W orkspace functions in Quick Start the same as if you selected W orkspaces from the
Syngistix application button (ball) in the ribbon.
Select a M ethod
A method controls instrument settings and how the instrument acquires and processes data in
an analysis.
Quick Start
Express Analysis: Use this command to display the Quick Start dialog so that you can turn on
the Plasma and "quickly" set up and run an analysis based on previously stored information.
Plasma Group
Plasma Control: Use this command to view the Plasma Control window. You use this window to
ignite and adjust the plasma, control the peristaltic pump and check instrument status.
Devices Group
Devices: Click Devices to display the dialog to control your devices; Pump, Autosampler, FIAS,
and Remote Trigger.
Probe Up/Down: Use this command to move the autosampler probe up or down, depending
on its current position.
Pump On/Off: Use this command to select options for the peristaltic pump. When you click
on this command, the Configure Pump appears, where you make your selections.
Flush Pump: Use this command to flush the pump.
Go to Wash: Use this command to go to the autosampler ___location of the wash solution. The
___location of the wash solution is selected in the method on the Sampler: Autosampler Wash page.
Go to Location...: Use this command to select the ___location where the autosampler probe will
move. When you click on this command, the Go To Location dialog appears.
Load Tray Use this command to move the autosampler probe up and then to the back left
position. This is the same as clicking on Load Tray in the Automated Analysis Control window.
Utilities Group
Diagnostics: Displays diagnostic information for Spectrometer, Plasma, Autosampler, and FIAS.
Scheduler: Displays the Scheduler dialog to set the automatic Start up and Shutdown times.
Plasma Cam: When you click the Camera icon the Plasma Camera window displays from
where you can view the Plasma.
Edit Group
Column Fill..: Use this command to fill a selected column in the Method Editor or Sample
Information Editor. When you click on this command, a dialog appears where you enter values
to fill the selected column.
Insert Rows: Use this command to insert an empty row into a table of parameters such as
those in the Method Editor or Sample Information Editor. Select a position in the line after the
one you want to insert and then select the command. A line will be inserted before the line
containing the cursor. All entries below the inserted line move down one position.
Delete Rows: Use this command to delete selected rows from a table. All entries below move
up respectively one position.
Cut: Use this command to remove selected text or values in a table and place in the Windows
clipboard.
Clear: Use this command to remove selected text or values in a table.
M ethod Group
Method: Use this command to view the Method Editor, where you enter analytical parameters.
New: Use this command to create a new method. The Create New Method dialog appears,
where you can select a set of plasma conditions in a new method for different types of
analyses, for example, organic or aqueous. Or, you can choose to use a copy of the active
method or another stored method as a starting point.
Open: Use this command to select a stored method for editing or performing manual analyses.
The Open Method dialog appears.
Save: Use this command to save changes to the active method. The first time you save a
Method, the Save As Method dialog will appear prompting you for a name. Note: If, for any
reason, a method is not ready to be saved, a check method dialog will appear.
Import Method: Use this command to import a method.
Check Method: Use this command to check for any problems or inconsistencies in the method.
Sort by...
Wavelength - Ascending/Descending: When the Method Editor Instrument page is
open, use this command to sort the elements in the method by the wavelength.
Analyte - Ascending/Descending: When the Method Editor Instrument page is open, use
this command to sort the elements in the method alphabetically by the element name.
Software Overview . 19
Element Symbol: When the Method Editor Instrument page is open, use this command to
sort the elements in the method alphabetically by the element symbol.
Function: When the Method Editor Instrument page is open, use this command to sort the
elements in the method by the function (as indicated by "analyte" or "internal standard").
Analyze Group
Analysis: Use this command to open the Manual and Automated analysis window.
Enable/Disable Analytes: Use this command to include or exclude an analyte from your
method in an analysis. When you click on this command, the Enable/Disable Analytes dialog
appears, where you can make your selections.
Automatic Export: Use this command if you want to automatically export data contained in a
results data set and write it into a file that can be read by many other programs, including
spreadsheet and database management programs. The Automatic Export dialog appears. The
export file contains ASCII data records.
Autosampler Load List: Use this command to open the Autosampler Loading List dialog to
view and print the list of solutions you need to fill the autosampler tray. The information shown
is taken from the active method and the current sample information file.
Spectra Group
Spectra: Use this command to change the number of panes and the colors that appear in the
Spectra Display window. You can also optimize colors for printing screens of this window in a 2-
column by 3-row format. When you click on this command, the Spectra Display Options dialog
appears.
Clear: Clears the display on the Spectra or Peaks window.
Calibration Group
Calibration: Use this command to view the Calibration Display window, which shows the
active calibration curves.
New Calibration: Use this command to clear the existing calibrations from the Calibration
Display window. You can generate a new calibration by analyzing the calibration standards.
Calibration Summary: When you are performing a Manual Analysis, use this command to
view a summary of the calibration data. When you click on this command, a calibration
summary is added to the information in the Results Display Window. (In an Automated
Analysis, the calibration summary appears automatically in the Results Display Window after
the last standard is analyzed, provided that this option is selected on the Options page of the
Method Editor.)
Recall Calibration...: Use this command to recall a stored calibration from the results library.
After you click on this command, select the results data set where the calibration is stored. If
several sets of calibrations have been run, the most recent one will be recalled.
Clear Calibration Blank: Use this command to clear the calibration blank concentrations from
the analysis. If multiple calibration blanks have been analyzed, all calibration blank
concentrations are cleared.
Clear Reagent Blank: Use this command to clear the reagent blank values for all analysis. If
multiple reagent blanks have been analyzed, all reagent blank values are cleared.
Edit Calibration: Use this command to display the Edit Calibration window where the active
calibration curve can be modified.
Ex am ine Group
Examine: (Spectra/MSF) Use this command after data is acquired and saved to view the
Examine Spectra window, where you can examine the spectra in detail, one element at a time.
You can use this window to overlay spectra and to select peak wavelength and background
points. You also use this window for Multicomponent Spectral Fitting (MSF) by creating models
for analytes and interferents. You must save the data in order to perform these functions in this
window.
Results Group
Results: Use this command to view the Results Display window, which shows the
measurements made on the current sample, the calculated concentration values, and statistical
information.
Clear: Clears the display.
Software Overview . 21
Options:
User Message: Use this command to print or save a message with your results. The
Message dialog appears, where you enter the message.
Analytical Header: Displays the Analytical header in the Results window.
Find: Displays the Find dialog to search within the Results window.
Reset Page Numbers: When information in the Results window is printing, use this
command to reset the page number of the next page to be printed to 1. This overrides the
usual situation where the page numbers are consecutive when the Results window is
printed.
Skip Line: In the Results window, use this command to add a blank line after the end of
the text. When the Results window is printed, it will contain the added space.
New Page: When information in the Results window is printing, use the command to force
a page to print, even if the page is only half filled with information. Usually, a page does
not print until it is completely filled.
Data Viewer: Launches the Data Viewer window containing your Results.
Reprint Data: Use this command to view the Reprint Data window. You use this window to
specify which results data you want to reprint.
Reprocess: Use this command to view the Data Reprocessing window. You use this window to
reprocess existing data.
Applications Group
Syngistix Offline: Use this command to run Syngistix Offline without the software controlling
the ICP. This allows the user to edit methods and reprocess the data.
Data Manager: Use this command to open Data Manager for reporting, data export, and
database maintenance.
ES Tools: (Displays in ES only) Use this command to open ES Tools application to Review and
Approve/Reject methods and samples.
Resources Group
Wavelength Table: Use this command to view the Wavelength Table window. You use this
window to select wavelengths when creating or editing a method or identifying interferences
viewed in the Examine Spectra window.
Periodic Table: Use this command to open the Method Periodic Table, where you enter
elements and wavelengths to create a new method or modify an existing method.
22 . Syngistix™ Software Guide
ICP Group
Click the appropriate button to change techniques from Continuous to Transient.
Note: The Transient Technique is not available on the Syngistix 4.0 ES version.
K eyboard Shortcuts
The following keyboard shortcuts are available in Syngistix.
Key Function
F1 Help Help
F2 ---
F3 ---
F4 ---
F5 Analyze Blank
F6 Analyze Standard
F7 Analyze Sample
F8 Cancel Analysis
F9 Plasma On/Off
2. Once this feature is set in User Setup, when logging in to Syngistix, a user checks the
Hide login upon initialization check box and logs in. Upon the next initialization,
Syngistix will login using the last logged in user.
3. To change back to show the login upon initialization, in the ball menu of Syngistix,
there is a menu item: "Show Login". Once selected, the login window with the check
box for hide login will be shown. User can then uncheck the box and login. Upon next
initialization of Syngistix will show the login screen.
Note: This setting does not apply to the Installer, Reconfigure, User Setup and Switch User. Meaning
that user would not see the check box.
24 . Syngistix™ Software Guide
Electronic signatures are required for critical operations, such as those operations which cause
data to be collected, administer security, or cause modifications to protected files.
What is an electronic signature?
An electronic signature as defined by 21 CFR Part 11 means a computer data compilation of
any symbol or series of symbols executed, adopted, or authorized by an individual to be the
legally binding equivalent of the individual's handwritten signature.
What is a signature point?
A Signature Point is a point in the software that requires a signature. The Signature Points are
pre-defined. The user has to enter their User name, Password (if this option has been selected)
and Reason for saving the method. They may also be able to add additional Comments if this
option has previously been selected by the Administrator.
Software Overview . 25
5. Make you selection for Require Signature and Prompt For Comments then click OK.
6. When done click Apply or click OK to save your entries and exit the dialog.
26 . Syngistix™ Software Guide
Note: Restricted access to functions outside of admin granted permissions are displayed to the user
as either grayed-out or an error message shall pop-up.
28 . Syngistix™ Software Guide
M essages
Use this dialog to print a message regarding the analysis in your results. You can also save this
message to the results library.
To display this dialog:
On the Results tab in the Results group click Options and select User Message.
Using this dialog:
1. Type the message in the dialog.
2. Check that you have the desired option(s) checked:
• If you select Print Message, the message will appear in the Results window and
be printed in the log.
• If you select Save Message, the message will be saved in the active results
library.
Software Overview . 29
Note: Double-clicking on an icon displays the appropriate screen. For example, double-clicking on the
Hardware icon takes you to Diagnostics, while double-clicking on the Plasma icon takes you to
Plasma Control.
User Name: Displays the User Name. Double-clicking on the user icon (to the left of User
Name) displays the User Details panel which displays the User ID, User name, Group
membership, and Permissions.
Detailed Status: This text field is only displayed when an operation displayed in the System
Status requires an additional detailed status.
Active data files: Lists the current Method, Sample Information File, and Data Set.
30 . Syngistix™ Software Guide
Diagnostic Status: The most recent diagnostic status from each piece of hardware
configured for the system next to the corresponding appropriate icon. Diagnostic Status will
also include an icon and status for scheduler.
Remote Client Status: Displays if the remote client is connected or not connected. Double-
click on the icon to display the Remote Access diagnostics page.
Note: You can drag the panel around the workspace and it will behave like a floating pane. To dock
the panel double-click anywhere in the pane and the pane is docked in the right-hand area of
the Syngistix workspace.
Note: If Data Storage is off, the Data Set name field will state: “Not saving data.” and will appear in
italics.
Status I cons
By double-clicking on the status icon for the Plasma, Spectrometer, or Autosampler, you can
get further information about the system component in the Instrument Diagnostics window.
By double-clicking on the status icon for Auto Shutdown/Startup, you open the Automatic
Shutdown/Startup dialog.
Software Overview . 31
Axial
Not Connected Connected Axial Plasma On Radial Plasma On Radial Plasma Error
Plasma Off Plasma Off Vertical and
Horizontal Axial
For instrument models with a vertically mounted torch, the icons have a different orientation
but the meaning is the same.
Spectrom eter Status Icons
System M essages
The System Monitor windows display the most recent messages pertaining to the system
component. To view a complete log of messages, refer to the Instrument Diagnostics Window.
32 . Syngistix™ Software Guide
Status Description and Value: This includes information on the Spectrometer model,
Current time, Operating mode, Connection mode, Control module version, Firmware and Kernal
version, Serial numbers, Gasses, Temperature, Water and Voltages the current status of the
instrument. To view all of the information, use the scroll bar.
Instrument Message History: This includes a log of all of the messages that have been
displayed in the System Monitor for the spectrometer. The most recent message is listed first.
All messages listed here pertain to the spectrometer hardware. Messages marked with a
question mark (?) indicate a "marginal" problem such as a temperature or voltage is too low or
Software Overview . 33
too high. Messages marked with an asterisk (*) indicate a "fatal" problem that would cause the
spectrometer to shut down. Refer to Operating Status Problems for common status problems.
For information on the different spectrometer error messages, refer to the Hardware Guide for
your spectrometer. To print this information, click on the Print button.
Configure IP: Click on this button to launch the Spectrometer IP Configure dialog. (This
is not available when the Simulation mode is configured.)
Note: This button only appears for spectrometers connected via Ethernet.
Advanced: Click this button to display a dialog describing the argon quick change feature.
Initialize: This button appears only for Simultaneous ICP spectrometers and is used to start
up the spectrometer when it is in standby mode.
Reconnect: Click on this button to reset communication between the system components if a
problem has occurred. For more information, see System Communication.
Print: Click on this button to print the instrument status information and the message history.
This information is useful for PerkinElmer service engineers in troubleshooting a problem.
IP Configure Dialog
This dialog enables you to set the IP address configuration for your spectrometer.
MAC Address: Enter the Media Access Control (MAC) Address that is specific to your
spectrometer and is a unique identifier. It is located on the spectrometer board, and on a
sticker that is located on the back of your instrument.
Get IP Configuration: Click the Get IP Configuration button to retrieve the IP configuration
from the spectrometer. The Status area displays the status of selected action.
Configuration Section: Network node configuration of the spectrometer.
IP Address: An identifier for a device on a TCP/IP network. Enter the IP Address when Static
IP configuration is selected.
Network Mask: Groups IP addresses together to form a sub net. Enter the Network Mask
when Static IP configuration is selected.
Gateway: IP address of your network Gateway. Enter the network address of your network
gateway when Static IP configuration is selected.
Device Name: The name used to identify your spectrometer rather than IP address, when
DHCP is selected. Enter the Device Name to identify your spectrometer when DHCP is selected.
Static IP: Click to select a fixed Internet Protocol address.
DHCP: Click to select Dynamic Host Configuration Protocol (DHCP), a protocol for assigning a
dynamic IP address on a network.
Set IP Configuration: Click this button to set the entered IP configuration into Syngistix and
optionally the spectrometer when the Spectrometer checkbox is checked.
Restore Defaults: Restores default values into all entry fields.
Note: This button does not configure the spectrometer. Only the dialog fields are affected.
Configuring IP
When you open this dialog, a default MAC address is entered into the MAC Address entry field.
The first four fields are populated with the best known starting address for spectrometers. The
last two are populated with zeroes. The MAC address will be persisted by Syngistix, and will only
require re-entry upon: Re-installation of Syngistix, or when connecting the PC to another
spectrometer. Default values for all other dialog fields are entered into the dialog. Those fields
are: IP Address, Network Mask, Gateway, Device Name, Static IP, and DHCP. Values for all
these fields are persisted by Syngistix.
The Syngistix checkbox is always checked and always disabled. Its purpose is to indicate that
Syngistix is always configured whenever the Set IP Configuration button is selected. The
Spectrometer checkbox is unchecked when the dialog is opened.
1. Before proceeding, enter the MAC Address for the spectrometer the first time
Syngistix is installed.
The MAC address is unique to the spectrometer and is located on the spectrometer
board, and on a sticker that is located on the back of your instrument.
2. Click Get IP Configuration once a valid MAC Address has been entered to retrieve
the configuration currently set into the spectrometer.
The configuration is displayed in controls within the Configuration group box. The
status display informs you of the operation sequence and the outcome.
Messages are displayed describing operations performed.
Note: The Status display is cleared upon entry of any value into any field.
Note: Check the Spectrometer checkbox to configure your spectrometer in addition to Syngistix. Only
the Device Name is required to configure Syngistix.
PC Setup
All PCs used with Ethernet spectrometers will have the same IP configuration for the network
card used for connection to the spectrometer:
Static IP address "64.1.3.2", Network mask "255.255.0.0", Gateway is not used and can be set
to "0.0.0.0", Device name is not used and can be set to blank.
3. Click the Change the argon tank button to put the instrument in standby so you can
change the tank.
This displays the Proceed now with changing the tank dialog.
36 . Syngistix™ Software Guide
Plasm a Page
This page displays the status information and the Instrument Message History for the plasma
generator.
Status Description and Value: This includes information on the generator model, base
module software and firmware versions, and the current status of the plasma generator. To
view all of the information, use the scroll bar.
Instrument Message History: This includes a log of all of the messages that have been
displayed in the System Monitor for the plasma. The most recent message is listed first. All
messages listed here pertain to the plasma generator. Messages marked with a question mark
(?) indicate a "marginal" problem such as a temperature or voltage is too low or too high.
Messages marked with an asterisk (*) indicate a "fatal" problem causing the plasma generator
to shut down. Refer to Operating Status Problems for common status problems. For
information on the different plasma generator error messages, refer to the Hardware Guide for
your spectrometer. To print the information, click on the Print button.
Save Log: Click on this button to select Black Box log or Incident log in the popup dialog.
Note: When a Black Box log file or Incident log file is uploaded and saved on disk two copies of the
file are saved: (1) a text file in the current format, and (2) a comma-delimited CSV file.
Software Overview . 37
Advanced: Click this button to display the Advanced Plasma Functions dialog. Here you
can do the following:
• Reset Emergency Plasma OFF setting
• Calibrate auxiliary and plasma torch gases.
• Change torch and injector adapter O-Rings. Reset the timer after replacing the O-rings.
• View instructions on fixing and/or preventing an axial optic overheating error.
Reconnect: Click on this button to reset communication between the system components if a
problem has occurred. For more information, see System Communication.
Print: Click on this button to print the status information and the message history. This
information is useful for PerkinElmer service engineers in troubleshooting a problem.
O-ring M aintenance
The torch o-rings have a recommended maximum lifespan of 300 insertions or 1 year of use,
whichever comes first. Worn o-rings may lead to difficulty when lighting the plasma and poor
performance and must be replaced.
1. Please replace the two torch o-rings with PerkinElmer part number N0791334 and
injector o-ring with PerkinElmer part number N0791333.
2. Once the o-rings have been replaced, click on RESET to remove this dialog from the
screen and reset the software.
3. Increase the ventilation rate (the ventilation rate must be at least 120 cfm).
The result of not correcting an overheating error will be the degradation of the axial optic flat,
shortening its lifetime, and requiring it to be replaced prematurely.
Status Description and Value: This includes information on the Autosampler model,
Instrument serial number, Control module version, Firmware version, and Tray file name. To
view all of the information, use the scroll bar.
Instrument Message History: This includes a log of all of the messages that have been
displayed in the System Monitor for the plasma. The most recent message is listed first. All
messages listed here pertain to the autosampler. Refer to Operating Status Problems for
common status problems. To print the information, click on the Print button
Firmware: Click on this button to install the firmware used when the current version of
Syngistix was developed.
Note: The Firmware button only appears if you have an autosampler that uses downloadable
firmware. Also, you must have administrator privileges for the local Windows Workstation. You
can check for such privileges under Start > Programs > Administrative Tools > User Manager.
Reconnect: If the autosampler has been disconnected, then reconnected; the autosampler
power was off, then turned back on when the software was started; or if you have selected a
Software Overview . 39
different type of autosampler, use the Reconnect button on the Autosampler page of the
Diagnostics window. For more information, see System Communication.
Print: Click on this button to print the status information and the message history. This
information is useful for PerkinElmer service engineers in troubleshooting a problem.
FI AS Page
This page shows important information about the flow-injection system that is useful for
troubleshooting and service purposes.
Status Description and Value: This information identifies your flow-injection system. You
should have this information available when you discuss problems with your PerkinElmer
service engineer.
Instrument Message History: This is a list of all the messages sent to and received from
the computer. This is very useful diagnostic information for the service engineer.
Reconnect: Use this button to reset the communication between the flow-injection system
and the computer.
Print: Use this to print the information shown in this window. This page displays status
information and the Instrument Message History for the FIAS.
40 . Syngistix™ Software Guide
Status Description and Value: This includes information on the DLL version, Firmware
version, Counter serial number, Sensor serial number, Data delay(s), Time per replicate(s),
Flow rate, and Counter calibration file. To view all of the information, use the scroll bar.
Instrument Message History: This includes a log of all of the messages that have been
displayed in the System Monitor for the Particle Counter. The most recent message is listed
first. All messages listed here pertain to the autosampler. Refer to Operating Status Problems
for common status problems. To print the information, click on the Print button.
Reconnect: Click on this button to reset communication between the computer and the particle
counter. You should do this only if the program was not able to communicate when it first loaded
or has lost communication. This could happen, for example, if power to the particle counter was
not turned on or the cable was not connected. For more information, see System Communication.
Print: Click on this button to select a printer and print the status information and the message
history. This information is useful for PerkinElmer service engineers in troubleshooting a problem.
Software Overview . 41
Status Description and Value: This includes information on the Server IP address, Server
port, and Client name, IP address. To view all of the information, use the scroll bar.
Remote Access History: This includes a log of all of the commands sent by the remote
client with the most recent listed first.
Print: Click on this button to select a printer and print the remote access command history.
This information is useful for PerkinElmer service engineers in troubleshooting a problem.
42 . Syngistix™ Software Guide
To perform analyses:
Use the tabs shown above to select the group of steps required for your analyses.
For information on the system installation, maintenance, and troubleshooting, refer to the
Hardware Guide for that instrument.
Performing Analyses Tab Results
7 Reports - Generating Reports • data from analyses collected and then printed
using Syngistix Data Manager
1 Set Up
2. Check Enable Syringe COM and select the COM port that has been automatically identified
as “Syringe (detected)”.
3. Close the Configure Syringe window and click on Initialize Autosampler.
2. If the ESI with prepFAST is not shown on the Autosampler Configuration screen, use the
Syngistix for ICP Reconfigure utility to select the correct autosampler.
3. Use the Flush at start of analysis check box to enable/disable the prepFAST Flush routine
that occurs at the start of an analysis or when resuming an analysis.
Performing Analyses . 47
prepFAST Method File: Selecting from standard prepFAST methods can be accomplished by first
selecting the desired Flow Rate then selecting the sample Loop Size and the maximum dilution
factor range. The specific name will change to match the prepFAST Settings that are selected.
Advanced: Use this selection when you desire to use a method other than the default methods
provided. The manual selection of a specific method will then be available in the FAST Method Control
window.
48 . Syngistix™ Software Guide
Before proceeding, be sure you have completed instrument setup as outlined in Set Up: Summary of
Steps.
Troubleshooting
If acceptable performance is not found with these tests, see the Hardware Guide for
troubleshooting performance problems. The performance tests can often pinpoint the cause of
the problem.
Performing Analyses . 49
Before you can analyze samples, you need: windows suitable for your analysis; one or more
methods; and a sample information file.
Note: The Workspace displayed when you close Syngistix is saved and redisplays when you reopen Syngistix.
- or -
If you are not using a sample information file, deselect the check box for Use Sample
Information. Then enter the autosampler locations in the Locations column.
50 . Syngistix™ Software Guide
6. Type individual locations or a range of locations. Use commas to separate the locations and
ranges. It is not necessary to enter the locations of blanks, QC's, check or calibration
solutions. Enter locations for these if you want them to be treated as a sample within the
analysis. Example: 10-15, 18, 20, 22 , 25-30.
7. The settings you have made can be saved in a workspace by selecting Save As from the
Workspace menu.
To select these items for manual analyses:
1. Select Workspace from the Application button then click on Open to display the Open
Workspace File dialog.
The group of windows (a workspace) that appears enables you to carry out your analysis.
The Manual Analysis Control window must appear in this workspace. Optional windows
include: Spectra Display, Results Display, Calibration Display, and Plasma Control.
If you do not select a workspace, you can select these windows individually from the
Windows and Tools menus. The selected windows can be saved as a workspace by selecting
Save As from the Workspace menu.
2. On the Analysis tab, in the Method group, click on Open to display the Open method
dialog to select a method.
3. If an appropriate method is not there, see Creating a Method.
4. A sample information file is optional. You may want a sample information file if you want to
enter all the sample information before an analysis begins. See Creating a Sample
Information File for details.
If you do not select a sample information file, the software uses the default file called
"Untitled." Be sure to open the Sample Information Editor and check that entries in the
"Untitled" file are appropriate for your analysis. If some entries are completed, but others are
not, the sample concentration may not be reported in sample units. See Sample Preparation
Parameters for details.
5. The settings you have made can be saved in a workspace by selecting Save As from the
Workspace menu.
Performing Analyses . 51
Before you can analyze samples, you need to set certain options in the control window that you are
using. These options are not specified in the method and include: specifying the results data set
where you will save data; specifying whether you want the results printed during the analysis;
specifying special automatic startup and shutdown options; and specifying automatic export of data.
For all analyses, to select options for the analyses:
1. On the Analysis tab, in the Analyze group, click on Analysis.
2. In the Automated Analysis window or the Manual Analysis window, click the check box
next to Save data to Results Data Set, click on the folder icon in the field box and in the
Select Results Data Set dialog that appears, type a new data set name, or select an
existing ones. If this data set already exists, new data will be added to it. When you select a
results data set name, the Save Data box is selected automatically (a check mark appears),
confirming that data will be saved.
Note: Archive result data sets periodically to avoid filling up space on the hard disk. For more information,
please refer to the Maintenance and Troubleshooting section of the Data Manager Help. To calculate
the amount of hard disk storage space that is required for storing result data sets, see Equation for
Calculating Disk Storage for Results.
3. To print a log of intensity counts, analytical results, and other information about the analysis,
select the Print Log During Analyses box.
For automated analyses only, to select other options:
1. If you want certain components to be automatically switched off when the analysis is
finished, first select the Automatic Shutdown box, then click on Set... to open the
Scheduler dialog. Complete this dialog, and click on OK.
2. If you want to enable Automatic Startup, use the above dialog to schedule an automatic
startup. You can also specify whether the plasma is to be ignited and if the pump is to begin
operating upon startup.
3. During the analyses, you can automatically export data contained in the results data set and
write it into a file that can be read by many other programs, including spreadsheet and
database management programs. To do this, select Auto Export, then click on Set... and
select the Export Designs. You must first create the Export Design(s) in the Syngistix Data
Manager. An export design defines a subset of data items that you want to export from a
data set. For more information, refer to Syngistix Data Manager Help.
4. On simultaneous ICP instruments only, you can select automatic wavelength realignment to
occur at regular intervals. Select the Auto Wavelength Realign box on the Automated
Analysis window and, then click on Settings to display the dialog to set a time interval.
5. The settings you have made can be saved in a workspace by selecting Save As from the
Workspace menu.
52 . Syngistix™ Software Guide
Before arranging samples in the autosampler using the autosampler loading list, you must have
entered all information for your samples and solutions in your method or methods and in the sample
information file if you have one.
For details on where to enter this information, see: Manual Analysis Control, Method Editor, and
Sample Information Editor.
To get samples and solutions ready for analyses:
Prepare the required samples and solutions according to your standard laboratory
procedures.
To load samples and solutions in the autosampler using the Automated Analysis Control window:
1. On the Analysis tab, in the Analyze group, click on Autosampler Loading List to see a
list of the locations of your samples and solutions.
2. Load samples and solutions in an empty tray.
3. In the Instrument tab, in the Devices group, click on Load Tray.
4. Place the loaded tray in the autosampler.
5. On the Instrument tab, in the Devices group, click on Go to Wash.
To load samples and solutions in the autosampler when the Manual Analysis window is open:
1. On the Analysis tab, in the Analyze group, click on Autosampler Loading List to see a
list of the locations of your samples and solutions.
2. Load samples and solutions in an empty tray.
3. On the Instrument tab, in the Devices group, click on Load Tray or press Shift-F11.
4. Place the loaded tray in the autosampler.
5. Click on the Go to Wash Loc. button in the Manual Analysis Control window.
Performing Analyses . 53
6 Analyze
Before analyzing samples, be sure you have performed all preliminary steps as summarized in
Performing Analyses: Overview.
There are three types of analyses:
Select how you will analyze samples from the options below.
• Automated Analyses, using an autosampler to analyze all samples and solutions.
• Manual Analyses, manually presenting samples and solutions to the instrument.
• Manual Analyses Using the Autosampler, requiring both manual operations and an
autosampler to analyze samples and solutions. In this case, often used for method
development, you want direct control of the autosampler, so the autosampler is just
holding samples for you.
Examining the Run List Before analyzing samples, you should check the run list. If any changes are
required, you must change either the method or the sample information
file, then rebuild the run list.
Calibrating and Analyzing Solutions and samples are analyzed. A calibration is performed according to
Samples your specifications, and you can recalibrate if desired.
Stopping and Restarting During the analysis, you may need to stop operations and restart the
analysis, according to these procedures.
Analyzing Additional Samples While an automated analysis is in progress, you can add samples to the
sample sequence, enter information on a new sample, or analyze additional
samples at the end of an analysis.
Note: During an analysis, the shutter automatically opens and closes for each sample. If you have an
extensive number of samples to analyze, however, you may wish to set the shutter to the open
position manually to increase analytical throughput. You do this in the Spectrometer Control Window.
Be sure to close the shutter when the analysis is complete.
Leaving the shutter in the open position with the plasma on could
lead to deterioration of the optics and eventual degradation of UV
performance. It is recommended that the shutter be closed when
analyses are not being performed.
54 . Syngistix™ Software Guide
M anual Analyses
Be sure you have performed all preliminary steps as shown in Performing Analyses: Overview.
Manual analyses are performed using the Manual Analysis Control window. Other windows such as
the Results window are optional.
To perform manual analyses:
Click on the desired step or use the buttons above.
During the analysis, you may need to stop operations and restart the analysis,
Stopping and Restarting
according to these procedures.
Note: In a manual analysis, the autosampler ___location in a sample information file is not used by the
software; therefore, you must use Go to A/ S Loc. to select the ___location each time you analyze a
sample.
Note: If you want different categories of information to appear in the Sample Details dialog, you need to
add the categories to the sample information file. For more information, see Customizing the Sample
Information Editor.
7 Generating Reports
If you saved data in a results data set (as requested in an analysis control window), you can use the
Syngistix Data Manager to generate reports in a wide variety of formats.
To start the Syngistix Data Manager:
On the Utilities tab, in the Application group, click on Data Manager.
or
On the task bar at the bottom of your screen, click on the Start button, select All Programs
PerkinElmer Syngistix for ICP Data Manager.
56 . Syngistix™ Software Guide
There are two ways to extinguish the plasma. You can extinguish the plasma manually or you can
extinguish it automatically using Automatic Shutdown. Automatic Shutdown can be selected in the
Scheduler dialog, which is accessed from the Automated Analysis Control page or using the Scheduler
command in the Utilities group in the Instrument tab.
Another mode is Automatic Startup, which can also be selected in the Scheduler dialog, as described
above. If you selected Automatic Startup to restart your system, this affects the procedures that you
follow when you shut down.
Note: If you have scheduled an Automatic Shutdown or Startup, you must leave the Syngistix software on.
Do not exit the software.
Note: Pressing the red Em ergency P lasm a Off button on the instrument allows you to shut off the
plasma directly and bypasses the software. This button can be used if the software hangs up or if
communication between the instrument and the computer is interrupted. Using this button does not
harm the instrument. If you use this button, you must reset the system before you can reignite the
plasma. To reset the system, be sure that the red button is in the out position, and select the R eset
Em ergency Off command in the System menu.
3. When the plasma is extinguished, the plasma off/on switch in the Plasma Control window
changes from blue to white and the peristaltic pump stops pumping solution to the plasma.
4. Proceed with this step depending upon the conditions of Automatic Startup.
If Automatic Startup is not being used.
-or-
If Automatic Startup has been selected and does not include turning on the plasma and the
pump.
Take the sample capillary out of the flush solution, and then run the pump for a few
minutes to clear solvent from the sample capillary and pump the spray chamber.
Release the clamp lever and remove the tubing. (This will increase the lifetime of the
pump tubing.)
Performing Analyses . 57
If Automatic Startup has been selected and includes turning on the plasma and the pump.
• Leave the sample capillary in the wash solution.
• If the level of the wash solution reservoir in the autosampler is above the spray chamber,
leave the peristaltic pump tubing clamped. This prevents the wash solution from being
siphoned into the spray chamber.
-or-
• If the level of the wash solution reservoir in the autosampler is below the spray chamber,
release the clamp lever on the pump tubing. This prevents the solution from being pumped
when the system automatically starts up.
• If desired, you can manually put the spectrometer on standby as described below.
To manually put the spectrometer on standby:
1. On the Instrument tab, in the Utilities group, click on Scheduler.
2. In the dialog, select Shutdown... and Immediately on OK. Be sure Put Spectrometer into
Standby is selected.
3. If the plasma has already been extinguished, be sure that the Wash before shutdown
option is not selected and that Turn off Plasma and Pump is not selected.
4. Be sure that you have enabled Startup and set the date and time.
58 . Syngistix™ Software Guide
Caution: If specific particle counting method parameters are changed from the predefined method, the
sample amount and timings might have to change.
3. Clicking the file open button opens the Open Method dialog which lists the available
predefined methods from the appropriate database.
4. Check the Analyze samples for particle counting/sizing box to use the particle counter
to acquire and analyze particle data with the given method.
This gives the users selections of which particle size and data formats are desired for the
analysis and they also can select the calibration file.
5. Select the file used to calibrate the sensor for particle counting/sizing. In the Calibration
file field, click the file open button , navigate to and select the desired Calibration file
(*.sns). The files are typically found in the following directory:
C:\Users\Public\PerkinElmer Syngistix\ICP\SystemFiles\AccessoryCalibration
6. Click the Open button.
7. Select a desirable Particle data format. This takes the counts and gives classification of
cleanliness. You can also add Additional sizes for your analysis.
8. Select if you want to Show counts for each replicate in results window.
9. Enter a Dilution factor.
Typically use a factor of 10.00.
10. Save your method.
60 . Syngistix™ Software Guide
7. In the Automatic Export dialog select Export Design 2, click the Open file browse
button , select the *.pxpx file and click the Open button. Click OK to accept the file
selection and close the dialog.
8. Make sure the Run list is populated with the correct samples.
9. When everything looks good, click the Analyze All button.
62 . Syngistix™ Software Guide
1. Getting Started
Ensure that your HTS system hardware is setup and configured.
1. On the Instrument tab click Devices.
2. Click the Pump tab.
3. Select the Tubing from the drop-down menu. The default tubing is black/black.
4. Select the Flush rate (mL/min). The default is 2.50 mL/min.
5. Select if you want to Enable tubing saver.
The tubing saver feature extends the life of the peristaltic pump tubing by operating the pump at
a low speed in alternating clockwise and counterclockwise rotations when the plasma is not on.
Note: You can also turn the Vacuum On or Off and the Valve to Inject or Load on the Instrument tab in the
Devices group on the ribbon.
2. I CP M ethod Settings
1. On the Analysis tab in the Method group click New.
The Create New M ethod dialog appears.
Performing Analyses . 63
7. Click the Sampler tab and click the HTS tab on the right.
The HTS parameter settings appear. The features of the Pump and Autosampler are
combined on this page. This consists of the HTS analysis settings and the Wash settings.
64 . Syngistix™ Software Guide
Estimated Analysis Time (s) Loop Size (mL) Loop Fill Time (s) Loop Wash Time (s)
5 -20 0.5 3 1
20 - 50 1 4 3
50 - 80 1.5 5 4
80 - 120 2 6 4
120 - 160 3 6 4
160 - 210 4 7 5
Wash settings
Never: No wash steps during the analysis. When this option is selected, the entry fields
for the options listed below are inactive.
Between Samples: The system washes the sample tube and probe after every solution
that it analyzes. Use the values in the Recommended Loop Parameters table for loop wash.
Only after samples whose concentrations exceed limits: The system washes the
sample tube and probe after it has analyzed a solution where the measured concentration
exceeds the value you select for Limit.
After every sample + extra time if sample concentrations exceed limits: The
system washes the sample tube and probe, after it has analyzed each solution, for the
time you select for Normal Time or the number of Normal Cycles. If the measured
concentration of a solution exceeds the value you select for Limit, the system will wash the
Performing Analyses . 65
sample tube and probe after analyzing this solution for an additional period of time that
you select for Extra Time or Extra Cycles.
Loop Wash: This parameter uses the vacuum of the HTS to rinse the probe and sample
loop.
Wash Location: The sample tray ___location of the wash solution.
Extra Time: Enter a value here if you want to set extra wash time after solutions where
the measured concentration exceeds the value you select for Limit.
M ethod Editor
You use the Method Editor to create a new method or to modify the parameters in an existing
method. You must have one or more methods to perform analyses.
W hat is a m ethod?
All analytical information needed to perform an analysis and report the results of an analysis is
contained in a method (and a sample information file, if it is used). You can use an existing
method as it is, modify an existing method to suit the purposes of your application, or create a
new method.
Modified or new methods must be saved in a methods library if you wish to use them at a later
date. You can delete, copy, or rename methods using the Data Manager application.
Tab/Pages Contents
Sampler Parameters for the Plasma, Peristaltic Pump. Autosampler wash, and
Particle Counter.
Process Directions to convert spectral data into intensity data, correct for
interferences and assign internal standards.
Options Remarks about the method and options for the results display, printed log,
and results data set.
Method Editor . 69
Using M ethods
There are several ways to get methods for your analyses. You can open an existing method
and use it as it is, modify it to suit your application, or create a new method.
Periodic Table
You can use this table to select the elements and their associated wavelengths for your
method. The elements and wavelengths that you select will automatically be entered on the
Method Editor Spectrometer: Define Elements Page. You can also enter elements and
wavelengths directly into the Method Editor.
-or-
• On the Method Editor Spectrometer: Define Elements Page, click on the
Periodic Table button.
To select elements and wavelengths for your method from the periodic table:
On scanning CCD ICP spectrometers, you can select any element at any wavelength. On
simultaneous ICP spectrometers, elements and wavelengths that are not available on the
detector are indicated by grey typeface.
1. Double-click on an element symbol. This enters the element and its default wavelength
directly into the active row in the table on the Method Editor Spectrometer: Define
Elements Page. The Active Row in Method Editor automatically increments to the
next row. Continue making your selections.
-or-
Click on an element symbol using the right mouse button. From the list of
recommended wavelengths, double-click on the desired value. (If you want to select
several wavelengths for one element, click on the wavelengths and then click on Enter
in Method.) This enters the element and the recommended wavelength directly into
the method. The Active Row in Method Editor automatically increments to the next
row. Continue making your selections.
2. When you have completed making your choices, click on the windows close box.
To select elements and wavelengths for your method from the alphabetical element list:
1. Select each element and its associated wavelength from the drop down lists. This
enters the element and its recommended wavelength directly into the active row in the
table on the Method Editor Spectrometer: Define Elements Page. The Active Row in
Method Editor automatically increments to the next row. Continue making your
selections.
2. When you have completed making your choices, click on the windows close box.
To change the values in any row:
• Change Active Row in Method Editor to the desired row, select the new element
and wavelength, and click on Enter in Method.
To search for elements at a particular wavelength or to choose wavelengths not on the
wavelengths list:
• Click on Wavelength Table and complete the entries as desired.
W avelength Table
You use this table to search for elements at a particular wavelength or to choose wavelengths
not on the recommended wavelengths list that is found on the Method Periodic Table.
Additional information such as intensities and BEC's are given for certain elements.
The elements and wavelengths that you have selected appear on the Method Editor
Spectrometer: Define Elements Page.
On scanning CCD ICP spectrometers, you can select any element at any wavelength. On
simultaneous ICP spectrometers, elements and wavelengths that are not available on the
detector are indicated by gray rows.
Tip: Double-click on a column header to sort the table by that parameter. For example you can sort
by element, state, wavelength, BEC, signal-to-noise, intensity, or any other parameter in the
72 . Syngistix™ Software Guide
column headers. Also see the table of references later in this topic. These publications were
used as sources for the Wavelength Table.
3. If the Center Wavelength entry field is not clear, double-click on this box and press
Delete to clear it.
4. Click on Search.
The specified wavelengths for that element appear in the table.
To display data for all elements:
1. Select All Elements in the Element to Include entry field, or click on the All button.
(All Elements means all elements in the wavelength table.)
2. Click on All Wavelengths or Recommended Wavelengths to specify what values
you want to see. If you have a simultaneous ICP spectrometer, you have an On
Arrays option as well. The On Arrays option will narrow down the search to just
those wavelengths that appear on the subarray.
3. Type a number in the Center Wavelength entry field or double-click on a wavelength
in the table.
4. Indicate the range in the Wavelength Range entry field. The default range is 0.5nm.
5. Click on Search.
All wavelengths that fall in the wavelength range appear in the table.
To copy an element and a wavelength into the method from the Wavelength Table:
If you opened the Wavelength Table from the Method Editor, you can copy entries directly into
the method.
1. Select the element and wavelength you want to add by clicking in that row.
Active Row in Method Editor defaults to the first blank row in the Method Editor
Spectrometer: Define Elements page. This is where the new information will be added.
2. If you wish to overwrite an existing Method Editor row, change Active Row in
Method Editor as desired.
3. Click on Enter Selected Wavelength in Method. The information is added to the
Method Editor.
To copy several elements and wavelengths into the method from the Wavelength Table:
If you opened the Wavelength Table from the Method Editor, you can copy entries directly into
the method.
1. Select the elements and wavelengths:
• To enter a range, click on a row and then hold down the Shift key and click on
another row. All of the rows in between will be selected.
• To enter information from noncontiguous rows, click on a row, then hold down
the Control key and click on additional rows to select them.
Active Row in Method Editor defaults to the first blank row in the Method Editor
Spectrometer: Define Elements page. This is where the new information will be added.
• If you wish to overwrite information in existing Method Editor rows, change Active
Row in Method Editor as desired. The row that you select will be where the first
element and wavelength in the group you selected in the Wavelength Table will
appear in the Method Editor.
2. Click on Enter Selected Wavelength in Method. The information is added to the
Method Editor.
74 . Syngistix™ Software Guide
To select a Copy of active method or Copy of another method to use as a starting point:
When creating a new method, it may be useful to start with a copy of the active method or
another stored method as a basis for creating the new method. By selecting Copy of
active method or Copy of another method, a copy of the method is opened in the
Method Editor called "Untitled." Modify the settings as needed, then save it under a
different name using Save As from the Save drop-down in the Method group.
To select a Copy of predefined method (Avio only) to use as a starting point:
Predefined methods as developed by the PerkinElmer Applications Group (for sequential
instruments only) are installed in Syngistix. By selecting Copy of predefined method, a copy of
the method is opened in the Method Editor.
1. Click on the Copy of predefined method radio button to use as a starting point.
2. Clicking the file open icon opens the Open Method dialog which lists the
available predefined methods from the appropriate database.
3. Select a method then click OK. The method name appears in the Create New Method
dialog selection box.
4. Click OK in the Create New Method dialog. This method opens in the Method Editor
as the active method with the name “Untitled”.
76 . Syngistix™ Software Guide
The methods Library database is stored where it was set up in User Setup. Select the
method you want then click the OK button.
An icon to the left of the method name indicates the current review status of the
method.
Approved
Rejected
If the Method Editor is open, the method name appears in the title bar. The method
name also appears in the Toolbar of the Syngistix main window, next to the Method
button. This is the active method, which controls your analysis. (You do not need to
open the Method Editor window to open an existing method.)
3. Use this method for your analysis with no modifications if desired. To change
parameters in this method, see Modifying a Method.
To open an existing method from a methods library (Non-ES)
1. On the Analysis tab, in the Method group, click on Open.
2. In the Open Method dialog, select the method you want from the list in the table,
then click on OK.
78 . Syngistix™ Software Guide
3. If the method you want is stored in a different methods library Database, click on
Browse and select the correct library ___location. Return to the Open Method dialog, and
select the desired method.
4. If the Method Editor is open, the method name appears in the title bar. The method
name also appears in the Toolbar of the Syngistix main window, next to the Method
button. This is the active method, which controls your analysis. (You do not need to
open the Method Editor window to open an existing method.)
5. Use this method for your analysis with no modifications if desired. To change
parameters in this method, see Modifying a Method.
To get a copy of a method associated with a stored results data set:
1. On the Analysis tab, in the Method group, click on Import Method.
2. In the Select Results Data Set dialog, select the results data set from the list in the
table, then click on OK.
If the Results data set you want is stored in a different Database library, click on
Browse and select the correct library ___location. Return to this dialog, and select the
desired Results data set from the list in the table.
3. When the Import from Results Library dialog appears, select the method you want
to import and then, at the bottom of the dialog, select the Method check box and
click on OK.
If the Method Editor is open, the method name appears in the title bar. The method
name also appears in the Toolbar of the Syngistix main window, next to the Method
button. This is the active method, which controls your analysis.
• Use this method for your analysis with no modifications if desired. To change
parameters in this method, see Modifying a Method. To save this method to a
method library, use Save or Save As... from the Save drop-down in the Method
group.
Method Editor . 79
M odifying a M ethod
You may want to make modifications to an existing method.
Note: If this file has been modified but not saved, the file name in the dialog header will have an
asterisk ( * ) displayed to the right of the name. Once the file is saved, the asterisk will be
removed.
To modify a method:
1. Open a method.
2. On the Analysis tab, in the Method group, click Method. Modify the entries as
desired on the Spectrometer pages, using the side tabs to view each page.
3. Display the remaining pages of the Method Editor by clicking on the tabs at the top of
the window and modifying the entries.
4. To save the changes, in the Method group click on Save to save the method with its
current name or from the Save drop-down list click Save As to display the Save
Method As dialog to save the method with a new name. The method is saved in the
Method database.
80 . Syngistix™ Software Guide
• Some options are associated with a check box. You may select as many of these as
you wish. When a check box is selected, it contains a check mark.
• Options for some parameters are contained in drop-down lists. Click on the arrow at
the right-hand side of the drop-down list to see the choices available.
• Spin boxes are often used for numerical parameter settings. To increase or decrease
the value, click on the appropriate arrowhead. You can also click on and type an
acceptable value.
• To enter information in a text box, click on the text box, then type the necessary value
or characters.
• To open another page of the Method Editor, click on the tab containing the name of
the page at the top or side of the window.
Tabs across the bottom of the Method Editor group parameters into several main
areas.
Saving a M ethod
You must save a method if you want to use it later. When you save a method, a copy of the
method is placed in the Methods database. Furthermore, a copy of the active method that was
used to obtain the results of your analyses is stored with the results data set.
Note: When you save a method, the software reviews all of the entries automatically. If it finds any
problems or inconsistencies, the Check Method message dialog is displayed to inform you of
the error.
Note: To save a method as a text file for making notations or printing, see P rinting a M ethod.
3. Clicking the file open icon opens the Open Method dialog which lists the available
predefined methods from the appropriate database.
P rinting a M ethod
You can print a method summary, which contains all of the parameters in the method. You can
also save a method summary in a text file, then open it in a text editor such as Notepad and
make notations or print selected sections.
To print a method summary:
1. Click on the Method Editor window to make it active. Note that the title bar of an
active window is a different color from other windows.
2. Right-click in the method then click Print from the list in the pop-up menu.
3. In the Print dialog that appears, check that the correct printer is shown. If you need
to select another printer or change other setup options such as the paper size, click on
Setup.
4. Click on OK to start printing.
Method Editor . 85
Detail of the Define Elements page showing entries included in an example method prepared
for a soils analysis.
Note: In the Transient technique, there is a six-analyte limit for entries in the table.
Method Description: This short description of your method will appear next to your method
name in the Open Method dialog. It will also appear in the Method Description field of the
Analysis Header displayed in the Results Display and Printed Log.
• Type up to 80 characters.
Symbol: This is the symbol of the element to be measured.
• To change or add an element, type the letters for the symbol in the entry field, or click
on Periodic Table. When the Periodic Table appears, select the desired elements.
Wavelength: This is the wavelength in nm that the Spectrometer will use to measure the
associated element.
To add or change a wavelength:
• Type an element symbol in the Symbol field to get the default wavelength for an
element.
86 . Syngistix™ Software Guide
-or-
• Type the value for the wavelength in the entry field.
-or-
• Click on Periodic Table. When the Periodic Table appears, select the desired
wavelength.
Note: In the Transient technique, the Active R ow In M ethod Editor counter does not go above
six enforcing the six analyte limit for entries in the table.
Name: This is the name that describes the element. The default entry is the element symbol
followed by the wavelength. No two elements in a method can have the same name.
• If you want to change the default name, type up to 20 characters, including spaces
and punctuation. For example, if you are determining analytes using different plasma
viewing modes or different plasma conditions, you may want to add information to the
default name such as "Al 396.152--Axial" or "Ca 317.933--0.8 neb".
Function: This is the role of the element in the analysis.
Analyte: The element's concentration will be determined based on a valid calibration.
Internal standard (Int. Std.): The element will act as an internal standard.
• Click on the text and select Analyte or Int. Std. from the drop-down list.
Note: For the Transient technique, the drop-down under the Function column have only the
Analyte choice.
Periodic Table
• Click on this button to display the Periodic Table, from which you can select elements
and their associated wavelengths for your method.
W avelength Table
• Click on this button to display the Wavelength Table, where you can search for
elements at a particular wavelength or choose wavelengths not in the recommended
wavelength list.
Spectral Settings
Purge Gas Flow
This is the spectrometer purge gas flow rate. The time taken to purge air from the spectrometer
depends on various factors, including how long the instrument has been in a low purge state.
Normal: A normal purge is used during routine operation.
High: The high purge is normally used during the analysis for wavelengths below 190 nm. A
high purge performed before an analysis clears the system of air, which contains moisture and
oxygen, before analyzing elements below 190 nm. See the Spectrometer Control window.
The default times are a minimum time of 0.5s and a maximum time of 2s. These values
are stored on a per-analyte basis in the method. In effect Auto integration means that
per-analyte min/max times are used (which may or may not be all the same).
When auto integration is used during an analysis, the actual integration time selected
for an analyte will be between the minimum and maximum times entered for that
analyte (it is possible in some cases for the actual integration time to be slightly longer
than the entered maximum time). This integration time is selected by the spectrometer
firmware based on analyte intensity. When the auto-integration summary table is
displayed at the end of a sample, and different limits have been entered for each
analyte (as this feature allows), the integration time shown for each analyte will be
within the entered limits specific for that analyte. This is how you can see that
integration times have been selected within limits on a per-analyte basis, based on the
entered min/max times.
To set the minimum or maximum time, use the Column Fill dialog.
• For manual control, click on Set... next to Manual. In the Set Manual Integration
dialog that appears, select the integration and read times for each analyte.
(Integration time is the time period in seconds in which the detector collects photons
before transferring the charge and reading out the signal. The read time is the total
measurement time in seconds per replicate.)
Delay Time: This is the number of seconds that elapse before the instrument begins to
measure the signal. Valid entry range: 0 - 999.
Replicates: This is the number of read cycles to be performed on each sample and
calibration solution. Valid entry range: 1 - 999.
Measure by: Only available for sequential spectrometers (for example, the Avio 200, Avio 220 Max,
Optima 7000/8000).
• Element - Selecting Measure by Element tells the spectrometer to stay at the
wavelength of the element for the number of Replicates selected. For example, if you
selected six (6) replicates for Cu and Pb it will measure Cu six times before it changes
wavelength to measure Pb six times.
• Replicate - Selecting Measure by Replicate tells the spectrometer to measure each
element once then repeat for the number of replicates. For example, if you selected six
(6) replicates for Cu and Pb, it will measure Cu once then change the wavelength and
measure Pb once for replicate one, then change the wavelength and measure Cu once
then change the wavelength to measure Pb once for replicate two until it completes
the cycle six times.
Method Editor . 89
Spectral Settings
Purge Gas Flow: This is the spectrometer purge gas flow rate. The time taken to purge air
from the spectrometer depends on various factors, including how long the instrument has been
in a low purge state.
Normal: A normal purge is used during routine operation when all wavelengths are greater
than 190 nm.
High: The high purge is normally used during the analysis for wavelengths below 190 nm. A
high purge performed before an analysis clears the system of air, which contains moisture and
oxygen, before analyzing elements below 190 nm. See the Spectrometer Control window.
By default, the survey window and auto integration window are set to the same wavelength
range. On simultaneous ICP spectrometers, this range is determined by the wavelength range of
the subarray on which the wavelength of interest falls. On scanning CCD ICP spectrometers, the
wavelengths are all directed to a single detector array, and the software sets the wavelength
range to default values.
On either type of spectrometer, you can adjust the wavelength range for the survey window or the
auto integration window. In some cases, it may be advantageous to set the auto integration window
to be smaller than the survey window. For example, if your interferent signal is higher than the
analyte signal, the auto integration time may be shorter than appropriate for your analysis. This is
because the software calculates the auto integration based on the highest signal, which, in this
example, would be the interferent. Therefore, you may want to limit the auto integration window to
exclude the interferent, so the software will calculate a longer integration time.
Note: In the Transient technique, the Auto Low er and Auto Upper columns in the table are not
used, since auto-integration is not used; however, these entries will remain enabled and
function as before.
Element and Wavelength: These view-only columns show the elements and wavelengths
selected for the current analysis. To change the element, click on the Periodic Table button
on the Spectrometer: Define Elements page. In the Periodic Table that appears, select the
elements and wavelengths desired.
Survey Lower and Survey Upper: This sets the wavelength range in which plasma
emission data is collected from the lowest to highest wavelength. The survey window must be
set equal to or greater than the auto integration window.
Auto Lower and Auto Upper: This sets the wavelength range in which the integration time
for the analyte is calculated.
When automatic integration is used, the software automatically sets the read time individually
for each analyte based on the signals of highest intensity. However, for some analyses, you
may want to select a smaller measurement range to exclude a strong interfering peak when
the integration time is being determined. This will give you improved signal-to-noise
characteristics for the analyte of interest.
Method Editor . 91
Plasm a Page
You use this page to set the plasma gas flows, RF power, viewing distance, and source
equilibration delay. These can be the same for all elements or different for one or all
elements. You can also specify criteria for monitoring the nebulizer back pressure.
Source Equilibration Delay: This is a delay in seconds, which can be used to allow the
plasma to stabilize after changes have been made to the plasma (source) conditions.
Plasma Conditions: You can assign the same gas flows, RF power, and viewing distance
values to all elements in the method or you can vary these values for each element
individually. If you have a dual-view instrument, you can also assign plasma view (axial or
radial) in this way.
Same for All Elements: Select this option to use the same gas flows, RF power levels,
viewing distances and plasma view for all elements.
Vary by Element: Select this option to vary the parameters for each element. Enter the
values you want in the table.
Note: In the Transient technique, the Vary by Elem ent radio button does not exist. This means
that the plasma conditions are the Same For All Elements. This forces Sam e For All
Elements (the default selection) to be always used.
92 . Syngistix™ Software Guide
Monitor Nebulizer Back Pressure: Click the checkbox to monitor the Nebulizer Back
Pressure from where you can specify that the system trigger an alarm when the nebulizer back
pressure is out of range.
Note: You can set up an audible alarm for when the nebulizer back pressure is out of range from the
Sound dialog.
Note: The following parameters have Colum n Fill dialogs that can be accessed by double-clicking on
the parameter's column header.
Plasma: This is the argon flow rate for the ICP torch plasma gas (also known as coolant or
outer flow). Valid entry range: 0 - 20 L/min. However, most torch designs will require a
minimum flow rate of about 10 L/min to achieve a stable plasma.
Aux: This is the argon flow rate for the ICP torch auxiliary gas. Valid entry range: 0 - 2.0
L/min.
Neb: This is the argon flow rate for the nebulizer or sample carrier gas. Valid entry range: 0 -
2.0 L/min. However, many nebulizer designs will allow a maximum gas flow rate of less than
2.0 L/min. See the information provided with your nebulizer to determine its maximum gas
flow rate.
Power: This is the amount of RF power delivered to the plasma discharge. Valid entry range:
750 - 1500 watts.
Method Editor . 93
View Dist: This is the nominal position within the plasma for the light that is measured by the
spectrometer. For radially viewed plasma, it is the distance from the load coil. For axially
viewed plasma, the 15-mm position represents the center of the plasma discharge.
Plasma View: If you have a dual-view instrument, this column is present. Plasma view refers
to the viewing position of the plasma torch, which can be set to radial or axial independently
for each analyte.
Radial: Light emitted from the side of the plasma passes through the torch slit and is directed
to the spectrometer optics.
Axial: Light emitted along the axis of the plasma is directed to the spectrometer optics. The
observation zone of the plasma is circular and the spectrometer views a column of light from
the central channel of the plasma.
Attenuated Radial or Attenuated Axial: These settings are available only for scanning
CCD ICP spectrometers. Use these settings when lower intensities are desired, for example, for
samples of high concentration that would normally saturate the detector and for sensitive
wavelengths, typically in axial mode.
Use this page to select the rate of sample flow, loop fill time and set the wash settings.
HTS analysis
Sample flow rate (mL/min): Select the rate in mL/min that the sample solution will be
pumped into the plasma during an analysis. As you change this value, the pump speed that
appears will be changed appropriately. The value range and ratio of pump rate to pump speed
depend on both the pump tubing and the pump model selected.
Loop fill (sec): Select or enter a time in seconds to fill the loop based on the loop
size. Allowed values depend on the tubing installed on the peristaltic pump.
Recommended loop parameters: Click this button to display a table of the recommended
loop parameters.
94 . Syngistix™ Software Guide
W ash settings
Never: No wash steps during the analysis. When this option is selected, the entry fields for the
options below are inactive.
Between Samples: The system washes the sample tube and probe after every solution that
it analyzes. Select a suitable option for Normal Cycles to tell the system how long to wash the
sampling system.
Only after samples whose concentrations exceed limits: The system washes the sample
tube and probe after it has analyzed a solution where the measured concentration exceeds the
value you select for Limit.
After every sample + extra time if sample concentrations exceed limits: The system
washes the sample tube and probe, after it has analyzed each solution, for the time you select
for Normal Time or the number of Normal Cycles. If the measured concentration of a solution
exceeds the value you select for Limit, the system will wash the sample tube and probe after
analyzing this solution for an additional period of time that you select for Extra Time or Extra
Cycles.
Loop Wash: This parameter pumps wash solution through the system. Allowed time depends
on the sample flow rate and length of the loop tubing.
Wash Location: The sample tray ___location of the wash solution.
Extra Time: Enter a value here if you want to set extra wash time after solutions where the
measured concentration exceeds the value you select for Limit. The system pumps wash
solution through the system using the FIAS program steps that you select below, for the
number of times you select here in addition to the number of times you select for Normal
Cycles. Use this option together with the option above: After all solutions + extra time if
solution exceeds limit.
Note: Analysis Time is defined as the time the instrument spends acquiring data.
Peristaltic Pum p
You use this page to select the rate of sample flow. You also select whether or not a sample
flush time should be added to the analysis delay time.
Note: You specify the type of autosampler that you are using when you install the software. If
needed, you can change this setting using the Reconfigure utility: on the task bar at the
bottom of your screen, click Start, Programs, PerkinElmer Syngistix, Reconfigure and use the
wizard to change the autosampler. To set the tray type, use the Options menu, Autosampler
command to display the Autosampler Configuration dialog.
Sm art Rinse
Select this option to enable SmartRinse. SmartRinse provides an automatic procedure to rinse
between samples in the minimal amount of time without contamination.
Note: Double click on the Concentration column to display the SmartRinse Concentrations Column Fill dialog.
Never
Select this option to be sure that no washes will be performed. When this option is selected
use the Wash Location spin box to specify the ___location of the wash solution in the
autosampler tray, usually zero (0).
4. In the Wash Location spin box specify the ___location of the wash solution in the
autosampler tray, usually zero (0).
2. Type the concentration limits you want for each analyte. The units shown are
Calibration Units.
These are selected from the Method Editor Calibration tab in the Calib Units and
Concentrations sub tab.
Note: The concentration parameter has a column fill dialog that can be accessed by double-clicking
on the column's header.
After every sam ple + ex tra tim e if sam ple concentrations ex ceed lim its
Select this option to increase the length of awash for any analyte when its concentration
exceeds a specified limit. The system washes the sample tube and probe, after it has analyzed
each solution, for the time you select for Normal Time or the number of Normal Cycles. If the
measured concentration or absorbance of a solution exceeds the value you select for Limit, the
system will wash the sample tube and probe after analyzing this solution for an additional
period of time that you select for Extra Time or Extra Cycles.
98 . Syngistix™ Software Guide
To wash after ever sample and add extra wash time if sample concentrations exceed limits:
1. In the Autosampler page, select After every sample + extra time if sample
concentrations exceed limits and then click on the Set... button.
The Extra Wash Concentrations Limits dialog appears.
2. Type the concentration limits you want for each analyte. The units shown are calibration
units. These are selected on the Calibration Units and Standard Concentrations page.
The total wash time will be the Normal time + Extra time selected on the
Autosampler Wash page.
When the concentration of any analyte exceeds the entered value, the wash time will
be increased by the amount of time you selected.
Note: The concentration parameter has a column fill dialog that can be accessed by double-clicking
on the column's header.
Frequency
Never: No wash steps during the analysis. When this option is selected, the entry fields for the
options below are inactive.
Between Samples: The system washes the sample tube and probe after every solution that
it analyzes. Select a suitable option for Normal Cycles to tell the system how long to wash the
sampling system.
Only after samples whose concentrations exceed limits: The system washes the sample
tube and probe after it has analyzed a solution where the measured concentration exceeds the
value you select for Limit.
After every sample + extra time if sample concentrations exceed limits: The system
washes the sample tube and probe, after it has analyzed each solution, for the time you select for
Normal Time or the number of Normal Cycles. If the measured concentration of a solution exceeds
the value you select for Limit, the system will wash the sample tube and probe after analyzing this
solution for an additional period of time that you select for Extra Time or Extra Cycles.
Wash Location: The sample tray ___location of the wash solution.
Normal Cycles: This parameter appears only with flow-injection techniques.
The system pumps wash solution through the system using the FIAS program steps that you
select below, for the number of times you select here.
Extra Cycles: Enter a value here if you want to set extra wash time after solutions where the
measured concentration exceeds the value you select for Limit. The system pumps wash
solution through the system using the FIAS program steps that you select below, for the
number of times you select here in addition to the number of times you select for Normal
Cycles. Use this option together with the option above: After all solutions + extra time if
solution exceeds limit.
Use FIAS steps: Select the first and last steps in the FIAS program that you want the system
to use for the wash cycle. You can set step 0, the Prefill step, as the first step in the wash cycle.
100 . Syngistix™ Software Guide
Steps to Repeat: Select a range of FIAS program steps that you want to be repeated, for
example, with the amalgam technique to make multiple injections. If you do not want to
repeat any steps, enter 0 for Number of Repeats.
Number of Repeats: This is the number of times the system will repeat the steps selected
for Steps to Repeat. If you do not want to repeat any steps, enter 0.
You use this page to set the particle size and data formats and a calibration file for the analysis.
A predefined method file is provided with the Syngistix software installation that is specifically
for Particle Counting ICP‐OES analysis.
Caution: If specific particle counting method parameters are changed from the predefined method,
the sample amount and timings might have to change.
Analyze samples for particle counting/sizing: Check this box to use the particle counter
to acquire and analyze particle data with the given method. This gives the users selections of
which particle size and data formats are desired for the analysis and also, they can select the
calibration file.
Calibration file: Select the file used to calibrate the sensor for particle counting/sizing. Click the file open
button , navigate to and select the desired file (*.sns) then click the Open button.
Particle data formats: Calculates results for the selected data format(s). This takes counts and
provides classification of cleanliness.
ISO 4406: When this box is checked, the processes used to determine oil cleanliness and
cleanliness classes are defined in the ISO 4406 table. ISO 4406 classification is based on
particle sizes >4µm(c), >6µm(c), and >14µm(c).
NAS 1638: When this box is checked, the processes used to determine oil cleanliness and
cleanliness classes are defined in the NAS 1638 table. NAS 1638 classification is based on
particle sizes 5-15μm(c), 15-25μm(c), 25-50μm(c), 50-100μm(c), and >100μm(c). The NAS
1638 particle numbers are differential, which means that the counts for the stated particle
figure range is reported.
102 . Syngistix™ Software Guide
SAE AS4059 Cumulative: When this box is checked, the processes used to determine oil
cleanliness and cleanliness classes are defined in the SAE AS4059 Cumulative table. SAE
AS4059 classification can be based on the >4µm(c), >6µm(c), >14µm(c), >21µm(c),
>38µm(c), and >70µm(c) particle sizes.
SAE AS4059 Differential: When this box is checked, the processes used to determine oil
cleanliness and cleanliness classes are defined in the SAE AS4059 Differential table. SAE
AS4059 classification can be based on the 6-14µm(c), 14-21µm(c), 21-38µm(c), 38-70µm(c),
and >70µm(c) particle sizes.
Particle sizes (mm): The Fixed and Additional particle sizes that will be analyzed based
on selections in the method.
Fixed: The particle sizes to be analyzed based on the selected data format(s).
Additional: Enter particle sizes to be analyzed in addition to the Fixed sizes.
Show counts for each replicate in results window: When this box is checked, it
shows replicate data for each sample in the Results log.
Note: The categories displayed depend on what is defined in the selection to the right. An example of
some of the categories are: >4 μm(c), >6 μm(c), >14 μm(c), >21μm(c), >38 μm(c), and
>70μm(c). Raw counts will not be shown in differential format.
Dilution factor (by volume): Enter the dilution factor (typically 10) used by the Particle Counter.
Method Editor . 103
P rocess Page
You use the entries on the Process pages to control the data processing part of the analysis.
Data processing involves converting spectral data into intensity data for each element and
correcting for spectral overlaps.
To display the Process pages:
1. Click on the Process tab on the top of the Method Editor window.
2. Click on the appropriate tab on the right-hand side of the window to select the pages.
• Spectral Peak Processing Page
• Spectral Corrections Page
• Assign Internal Standards Page
• Perform Internal Standards Checks
F'n (Function): This view-only column shows the action that the instrument will take for this
element. To change the parameter, use the entry field on the Spectrometer: Define Elements
page.
A = Analyte
IS = Internal Standard,
Analyte: This view-only column shows all the elements selected for the current analysis. To
change the parameter, use the entry field on the Spectrometer: Define Elements page.
Peak Algorithm: Select the mathematical algorithm that will be used to process the
analytical data on this item.
Note: In the Transient technique, the P eak Algorithm column drop-down choices contain only two
choices, P eak Ht and P eak Area.
Peak Area: The system uses the sum of the intensities recorded by the pixels on the detector
used for the read. The number of data points used is defined by the Points Per Peak entries on
this page. Since the total number of data points for each spectrum increases by a factor of four
104 . Syngistix™ Software Guide
when spectral profiling is turned on, you have to use four times as many points/peak to
measure the same area under the peak if spectral profiling is on than you would if spectral
profiling were off. You also must also quadruple the amount of time allowed for this to occur.
Peak Height: If you are not using spectral profiling, the number that you enter in Points Per
Peak defines the region that the software will search in order to locate the peak maximum. For
example, if you entered 5 in Points Per Peak, the software will search 5 points around the
calibrated center. When the software finds the point that produces the highest intensity, that
point will be defined as the Peak Height.
If you are using spectral profiling, the peak height is determined in different ways depending
on the number of points chosen:
1 point: uses theoretical wavelength or wavelength calibration point
2 points: uses highest of the 2
3 or 4 points: 3 point parabolic fit
5 or more points: 5 point cubic fit
The total number of data points for each spectrum increases by a factor of four when you use
spectral profiling. Therefore, if spectral profiling is on, you have to use four times as many
points per peak to define the same search region if spectral profiling is on than you would if
spectral profiling were off. You also must also quadruple the amount of time allowed for this to
occur.
Note: This parameter has a Column Fill dialog that can be accessed by double-clicking on the
parameter's column header. In the Transient technique, the MSF choice is not displayed.
Note: This parameter has a Column Fill dialog that can be accessed by double-clicking on the
parameter's column header.
Method Editor . 105
Spectral Corrections
You use this page to select the corrections to be made for spectral overlaps and shifting
background emission. Two kinds of overlap correction are possible, Interelement Correction
and Multicomponent Spectral Fitting.
Note: In the Transient technique, the section at the bottom of the Spectral Corrections page
containing IEC M odel and M SF M odel is hidden. Also, the Overlap Correction drop-down
contains only one choice, None (the IEC choice is eliminated). Since there is only one choice
for Overlap Correction, the corresponding column fill dialog is not used (double-clicking on
the column header has no effect).
F'n (Function): This view-only column shows the action that the instrument will take for this
element.
A = Analyte
IS = Internal Standard
To change the parameter, use the entry field on the Spectrometer: Define Elements page.
Element: This view-only column shows all the elements selected for the current analysis. To
change the parameter, use the entry field on the Spectrometer: Define Elements page.
Overlap Correction: Select a mathematical method that will be used to process the
analytical data on this item for spectral overlaps. It is possible to use one, two, or all three
settings in a method, although each individual element can only use one setting. The selections
that appear for Overlap Correction depend upon the peak algorithm that you selected on the
Method Editor Process: Spectral Peak Processing page, as shown below.
If the Peak Algorithm is: Then, Background Correction is:
Note: This parameter has a Column Fill dialog that can be accessed by double-clicking on the
parameter's column header.
Background Correction: Select a method that will be used to correct for background
changes for this element.
Auto: (Default) Dynamically creates a background correction spectrum for each ICP replicate
and/or average spectrum with no user interaction required using a propriety PerkinElmer algorithm.
None: No background correction will be made for this element.
1-point: One-point background correction will be made for this element (using BGC1).
2-point: Two-point background correction will be made for this element (using BGC1 and
BGC2).
MSF (Multicomponent Spectral Fitting): A multiple linear regression is done to fit the
spectra from the analysis to predetermined models. See Examine Spectra/MSF window for
more information. This option is automatically selected if MSF was selected as Peak Algorithm
on the Process: Peak Algorithm, Points/Peak page.
Note: This parameter has a Column Fill dialog that can be accessed by double-clicking on the
parameter's column header.
BGC1 (Background Correction Point 1): This entry is dimmed unless 1-point or 2-point
background correction is selected. It sets the offset from the wavelength selected on the
Spectrometer: Define Elements page to be used for the first background point.
• Type a number for the offset. BGC1 can be on either the left or right side of the peak
wavelength. If you wish to enter a negative offset to specify a point on the left side of
the peak wavelength, type a minus sign (-) and then a number.
- or -
• You can select background points in the Examine Spectra/MSF window. For more
information, see Using the Background Correction Point Option.
Note: This parameter has a Column Fill dialog that can be accessed by double-clicking on the
parameter's column header.
BGC2 (Background Correction Point 2): This entry is dimmed unless 2-point background
correction is selected. It sets the offset from the wavelength selected on the Spectrometer:
Define Elements page to be used for the second background point.
• Type a number for the offset. BGC2 can be on either the left or right side of the peak
wavelength. If you wish to enter a negative offset to specify a point on the left side of
the peak wavelength, type a minus sign (-) and then a number.
Method Editor . 107
Note: This parameter has a Column Fill dialog that can be accessed by double-clicking on the
parameter's column header.
Note: In the Transient technique, the Internal Standards and Internal Stds Checks tabs are
hidden, since internal standards are not supported.
Note: This parameter has a Colum n Fill dialog that can be accessed by double-clicking on the
parameter's column header.
W ash solution contains the internal standard(s) – for use w ith SmartRinse
When Internal Standardization is used and Smart Rinse is enabled you use the Wash solution
contains the internal standard(s) check box to define whether or not internal standards
are present in the wash solution.
Check Wash solution contains the internal standard(s) when internal standardization is
used and the internal standard is present in the wash solution.
When this option is checked internal standards will not be listed as elements that can be
monitored on the Smart Rinse Concentration Limits dialog. During a wash internal standard
correction will continue with the internal standard ratio being updated during the wash.
Uncheck Wash solution contains the internal standard(s) when internal standardization is
used and the internal standard is NOT present in the wash solution. When this option is
unchecked, internal standards will show up in the list of elements that can be monitored for
Smart Rinse. Internal standard correction will continue during the wash; however, the internal
standard ratio is not updated, but rather the last ratio determined will be used throughout the
wash.
108 . Syngistix™ Software Guide
Note: When SmartRinse is enabled on the Sam pler > Autosam pler page of the Method Editor,
internal standard limits are always reported as a percent, regardless of what is selected on the
P rocess > Internal Standards page.
Note: The Dilute and Reanalyze action is only available when an ESI with prepFAST is installed and
configured.
Method Editor . 109
Note: You can select to have a sound played when an Internal Standard Check fails from the Sound
dialog.
Note: If you have an ESI with prepFAST installed and configured you can also use this page to apply
a dilution if an upper or lower internal standard check fails.
Select a failure action to be performed when the measured concentration exceeds the lower
limits:
Dilute and Reanlayze: This option is only available if an ESI with prepFAST is installed
and configured. When Dilute and Reanalyze is selected you must also specify a dilution
factor. When this action is selected the sample will be reanalyzed by the factor you
specified.
Continue: When this action is selected the system prints a failure message, then
continues with the analysis.
Next Method: When this action is selected the system prints a failure message; the
current method is stopped; and the system proceeds to the next method, if any. If there is
no next method, the system stops the analysis.
Stop: When this action is selected the system prints a failure message and stops the
analysis.
110 . Syngistix™ Software Guide
Alarm and Pause: When this action is selected the system prints a failure message; an
alarm is activated; and the analysis pauses. At this point, you will get an option to stop or
continue the analysis.
To apply a dilution if an Upper or Lower Internal Standard Check fails (only for ESI
with prepFAST systems)
Note: If Internal Standard Checks and Sample Limit Checks are defined in your method and both
checks fail, then Sample Limit Checks will always take priority.
1. Use the Internal Standard Limits table to define Internal Standard Checks.
2. For the Lower Limit failure action use the reanalyze spin box to define the number of
times to reanalyze a solution after a lower limit is exceeded. You can specify a value
from 0 to 3. The default is 1.
3. Select Dilute and Reanalyze: When Dilute and Reanalyze is selected you must also
specify a dilution factor.
4. For the Upper Limit failure action use the reanalyze spin box to define the number of
times to reanalyze a solution after an upper limit is exceeded. You can specify a value
from 0 to 3. The default is 1.
5. Select Dilute and Reanalyze: When Dilute and Reanalyze is selected you must also
specify a dilution factor.
Note: If both the upper and lower limits are exceeded, the action defined for the lower limit will take
place.
Note: If a failure of a limit persists, the dilution action will only occur 3 times before continuing on to
the next sample.
In the example below, the internal standard Y, has limits of 90% and 101%. If the measured
concentration exceeds the lower or upper limits, the sample will be reanalyzed by a factor of
2X or 7X respectively.
Tim e Processing
Use this dialog to select, for each analyte, how time-based peaks are processed. You can
select, via the drop-downs, Peak Ht. or Peak Area processing (under the Peak Algorithm
column), and the number of points for Savitsky-Golay smoothing for peak height (choices of
None, 5, 9, 19, or 37 under the Smoothing Points column).
F'n (Function): This view-only column shows the action that the instrument will take for this
element.
Method Editor . 111
A = Analyte
IS = Internal Standard,
To change the parameter, use the entry field on the Spectrometer: Define Elements page.
Element: This view-only column shows all the elements selected for the current analysis. To
change the parameter, use the entry field on the Spectrometer: Define Elements page.
Peak Algorithm: Select the mathematical algorithm that will be used to process the
analytical data on this item.
Peak Area: The system uses the sum of the intensities recorded by the pixels on the detector
used for the read. The number of data points used is defined by the Points Per Peak entries on
this page.
Peak Height: The number that you enter in Points Per Peak defines the region that the
software will search in order to locate the peak maximum. For example, if you entered 5 in
Points Per Peak, the software will search 5 points around the calibrated center. When the
software finds the point that produces the highest intensity, that point will be defined as the
Peak Height.
Smoothing Points: Points used to smooth peak using Savitsky-Golay algorithm prior to
calculation of peak height. When measuring Peak Height signals, you may want to smooth the
signal to average out noise before measuring the height. This setting has no effect when
measuring peak area. It also has no effect of the graphical display of transient peak signals.
112 . Syngistix™ Software Guide
Calibration P ages
You use the Calibration pages to define calibration standards and concentrations and to select
parameters such as the type of calibration equation and the autosampler locations for blanks
and standards. You also select how blanks will be used, and whether or not to use a stored
calibration.
To display the Calibration pages:
Click on the Calibration tab on the top of the Method Editor window.
Calibration Pages
Click on the appropriate tab on the right-hand side of the window to select these pages:
• Define Standards Page
• Calibration Units and Standard Concentrations Page
• Calibration and Reagent Blank Usage Page
• Calibration Equation and Sample Units Page
• Initial Calibration Options Page
• Multiline Calibration Page
• Recalibration Page
Define Standards
You use this page to select the IDs and autosampler locations that you want to use for the
blanks, standards, and other calibration solutions.
Note: The screen shot below shows the Define Standards page when an ESI autosampler with
prepFAST is installed and configured.
Click here for an example of generating a calibration curve using a single stock solution (only
for ESI with prepFAST systems).
Method Editor . 113
Method of Additions: Check this option to analyze samples using method of additions.
When Method of Additions is checked a drop-down list of method of additions equations
becomes enabled. From the drop down select the appropriate method of additions equation to
use in your method. You can select from the following equations: Method of Additions, Sample
Intercept, Method of Additions, Calculated Intercept, Method of Additions Calibrate. Please
note that the equation you select here will be applied to all analytes specified in your method.
Click here for more information on Method of Additions.
Note: Method of Additions is disabled when the prepFAST system is installed and configured.
ID: This is the name that you give to each calibration solution. It will be printed on the log
and saved in the results data set. If you do not type a name, the system uses pre-set IDs such
as Calib. Blank, Calib Std 1, etc.
A/S Location: This is the autosampler ___location you wish to use for each calibration solution.
For autosampler trays that have multiple size tube capacities, the larger containers located in
positions 1 through 8 typically are used for blanks, calibration standards, and QC samples, if
any. The next available autosampler ___location is automatically assigned by the software when a
new calibration blank, calibration standard, or reagent blank ID is entered. The user may
modify the settings.
If you have installed and configured the ESI with prepFAST system use this column to
specify the ___location of your stock standards for each calibration point.
Note: If Method of Additions is checked, the Autosampler Locations are automatically filled in.
Dilution Factor: Use this column to specify the Dilution Factor to be applied by the prepFAST
for each calibration point.
Note: This column is only displayed when an ESI w ith prepFAST system is installed and configured.
Calibration Blank 1-5: You can use up to 5 calibration blanks. The calibration blanks are
analyzed before the standards in an automated analysis. How the calibrations blanks are used
in the analysis is defined on the Blank Usage page. (It is useful to have 5 calibration blanks
available, for example, if you need to create a blank to match each matrix in each standard.)
Type the ID for each calibration blank.
Internal Standard Blank: If you have entered an internal standard, this option appears on
the bottom of the scrolling list of Calib Blanks. (You may need to scroll to reach it.) If you
114 . Syngistix™ Software Guide
select an internal standard blank for the method, you decide which internal standards it is used
for on the Blank Usage page.
Type the ID for the internal standard blank.
Calibration Standard 1 - 30: You can use up to 30 calibration standards. These standards
will be analyzed in sequence (following the calibration blanks) in an automated analysis,
beginning with Calibration Standard 1.
1. Type the ID for each calibration standard.
If the ESI with prepFAST system is installed and configured you need to specify the
Dilution Factor to be applied to each calibration standard. The autosampler position
for each calibration standard defines the ___location of the stock standard from which the
dilutions will be made.
2. Assign the separate standards on the Calibration > Define Standards tab page of
the Method Editor.
3. Type 1 as the Dilution Factor for the standards you just entered in step 1.
4. Click on the Define Stock Std. Concentrations button.
5. On the Define Stock Standard Concentrations dialog enter the concentrations of each
standard.
6. Click OK to close the Define Stock Std. Concentrations dialog.
Note: Calibration Standards do not appear if Method of Additions is checked. If Method of Additions is
checked, then Additions 1-30 appear in place of Calibration Standards 1-30.
Note: When you select Method of Additions, the software assumes that the aliquots of sample
containing the additions (addition 1, addition 2, etc) immediately follow the original sample in
the autosampler tray. If there are two or more samples to analyze, each sample has its own
additions. The samples should be placed in the autosampler in the following order: blank,
sample, A1 (sample + addition 1), A2 (sample + addition 2), etc. You run a blank for the first
sample only. This blank will be used for all other samples.
Reslope Standard: You use the reslope standard to make small corrections to the slope of
the calibration curve using a single calibration standard following small changes in instrumental
conditions.
Note: You must also schedule when the Reslope Standard should be analyzed. You schedule the
Reslope Standard using the Recalibrate Before parameter in the Sample Information Editor.
If the ESI with prepFAST system is installed and configured you need to specify the
Dilution Factor to be applied to the reslope standard.
Reagent Blank 1-5: You can use a reagent blank to compensate for differences in
composition between the reagents used to prepare the samples and those used to prepare the
calibration standards. Reagent blanks are analyzed immediately after the calibration standards
Method Editor . 115
in an automated analysis. The reagent blank concentrations measured are subtracted from all
subsequently analyzed samples. If multiple reagent blanks are analyzed, their concentrations
are averaged and the average concentration is subtracted from each sample.
2. In the A/S Location column specify the ___location of your stock standard(s) for each
calibration point.
3. Use the Dilution Factor column to specify the desired Dilution Factors to be applied
for each calibration point.
4. Click on the Define Stock Std. Concentrations… button. The Define Stock Std.
Concentrations dialog displays.
5. Specify the concentration of the analytes in the Stock Standard solution as shown in
the screen shot below:
116 . Syngistix™ Software Guide
Note: The significant digits used to specify the Stock Std. Concentrations may affect the precision of
the system calculated values. F1.
Note: If you have an ESI with prepFAST installed and configured this page is read-only.
Detail of the Calibration Units and Standard Concentrations page showing entries included in
an example method prepared for a soils analysis.
Analyte: This view-only column shows all the elements designated as analytes for the current
analysis. To change the parameter, use the entry field on the Spectrometer: Define Elements
page.
Calib Units: This column shows the units in which the concentrations of your calibration
solutions/addition solutions are expressed.
Note: If you have an ESI with prepFAST installed and configured this column is read-only.
To change the units for an analyte, select an option from the drop-down list.
Note: This parameter has a Column Fill dialog that can be accessed by double-clicking on the
parameter's column header.
Method Editor . 117
Note: If you have an ESI with prepFAST installed and configured this column is read-only.
To enter or change the standard concentration for an analyte, type the new
concentration in the entry field.
To clear the standard concentration for an analyte, click on the entry field and press
Delete.
Note: This parameter has a Column Fill dialog that can be accessed by double-clicking on the
parameter's column header.
F'n (Function): This view-only column shows the action that the instrument will take for this
element.
A = Analyte
IS = Internal Standard
To change the parameter, use the entry field on the Spectrometer: Define Elements page.
Element: This view-only column shows all the elements selected for the current analysis. To
change the parameter, use the entry field on the Spectrometer: Define Elements page.
Use Calibration Blank: This column shows which calibration blank should be used as part of
the calibration for this element. Having multiple calibration blanks allows you to select different
calibration blanks for different elements to correct for differences in baseline of each blank
solution. The calibration blank is usually analyzed before the standards.
The way in which the calibration blank is treated in the calibration is based on the calibration
equation. For more information, see Calibration and Calculations.
• To change the calibration blank for one element, select an option from the drop-down
list.
Note: This parameter has a Column Fill dialog that can be accessed by double-clicking on the
parameter's column header.
Subtract Reagent Blank: This column allows you to use reagent blanks to correct for
variations in analytes. The normal way of using a reagent blank is to subtract the results for all
elements. By turning off reagent blank subtraction for certain elements that you know are not
present in the reagent blank, you can reduce the noise or bias that subtracting a near-zero
reagent blank concentration would otherwise add to a measurement. The column is active only
if one or more reagent blanks have been defined on the Define Standards page.
Note: This parameter is disabled if you checked M ethod of Additions on the Define Standards page.
Note: This parameter has a Column Fill dialog that can be accessed by double-clicking on the
parameter's column header.
Method Editor . 119
Note: If you checked M ethod of Additions on the Defined Standards page, then the Calibration
Equation cells are read-only. The Calibration Equation that is displayed for each element, when
Method of Additions is enabled, is the equation that is selected on the Define Standards page.
F'n (Function): This view-only column shows the kind of action that the instrument will take
for this element.
A = Analyte
IS = Internal Standard
To change the parameter, use the entry field on the Spectrometer: Define Elements page.
Element: This view-only column shows all the elements selected for the current analysis. To
change the parameter, use the entry field on the Spectrometer: Define Elements page.
Calibration Equation: This column shows the calibration equation used to process the
analytical data on this item, defining the relationship between intensity and concentration for
your samples. See Calibration and Calculations for further details.
Note: If you checked M ethod of Additions on the Define Standards page, then the Calibration
Equation cells are read-only. The Calibration Equation that is displayed for each element, when
Method of Additions is enabled, is the equation that is selected on the Define Standards page.
Linear-thru-zero: This creates a linear calibration curve, but forces the curve through the
origin of the graph.
Linear equations are used when you expect a linear relationship between concentration and
intensity. Generally, this is 4 to 6 orders of magnitude greater than the detection limits and will
depend on wavelength region and your sample matrix. In this equation, the blank is subtracted
from all solutions and included in the calculation of the calibration curve. The calibration curve
is forced to go through zero intensity and zero concentration.
Linear (Bracketing): This is a linear calibration technique designed for use over a restricted
concentration range. The calibration is performed with at least two standards that bracket the
calibration range of interest. The use of a blank is optional. If you use a blank, it is subtracted
from all solutions, but is not included in the calculation of the calibration curve.
Non-linear (Non Lin, Calc Int): Non-linear equations are used when you expect your
sample concentrations to be outside of the linear range of the technique. This option covers
the widest concentration range and requires that you use a blank and at least three standards.
In this equation, the blank is subtracted from all solutions and included in the calculation of the
calibration curve. The intercept with the intensity axis is calculated rather than fixed at zero
intensity and zero concentration.
Non-linear (Bracketing): Non-linear equations are used when you expect your sample
concentrations to be outside of the linear range of the technique. Bracketing is a calibration
technique designed for use over a restricted concentration range. The calibration is performed
with at least three standards that bracket the calibration range of interest. The use of a blank
is optional. If you use a blank, it is subtracted from all solutions, but is not included in the
calculation of the calibration curve.
Weighted Linear (Wt. Lin): When working at low level concentrations it provides an
alternative calibration scheme that weighs the low standards to a greater degree.
Note: This parameter has a Column Fill dialog that can be accessed by double-clicking on the
parameter's column header.
Sample Units: This column shows the units in which the sample results are expressed.
Conversion from sample results determined in Calib Units to results expressed in Sample Units
involves corrections made for weight, volume, and dilution information supplied for samples in
a Sample Information File (or the Sample Details dialog in a manual analysis), e.g. converting
from mg/L to mg/kg. Corrections are also automatically made for converting units with order-
of-magnitude differences, e.g. converting mg/L to µg/L.
To change the units for an analyte, select an option from the drop-down list.
Note: This parameter has a Column Fill dialog that can be accessed by double-clicking on the
parameter's column header.
You can select either Weight/Volume units or Weight/Weight units. There are, however, some
restrictions on using combinations of certain Calib Units with certain Sample Units with respect
to information that needs to be supplied in the Sample Information File (SIF) for each sample.
Failure to include the proper information with samples will cause sample results to be reported
in Calib Units only. See Sample Preparation Parameters for more details about the sample
quantity information required in the Sample Information Editor.
To select your own sample units, the units available in the drop-down lists are stored in a file
called units.inix located in C:\Users\Public\PerkinElmer
Syngistix\ICP\SystemFiles\Configuration. You can use any text editor to add units to the file.
You can also rearrange the units in the file so that those used frequently are on the top of the
list. The units.inix file contains information on the format and contents of the file. If the
units.inix file contains improper information, the software may fail.
Method Editor . 121
Max. Decimal Places: This column shows the maximum number of figures to the right of
the decimal point that are displayed for the concentrations reported in sample units or
calibration units.
It is possible that the final result will not include the number of decimal places specified here,
depending on the value that is specified for Max. Significant Figures. In general, when the
result is small, the Max. Decimal Places value is used. However, when the result is large, the
Max. Significant Figures is used.
Example 1
Max. Decimal Places = 3, Max. Significant Figures = 2
Calculated Concentration: 11.001
Reported Concentration: 11
The calculated concentration has three decimal places, but it exceeds the maximum
number of significant figures. Therefore, the result is reported as 11 with two significant
figures.
Example 2
Max. Decimal Places = 3, Max. Significant Figures = 4,
Calculated Concentration: 0.03587
Reported Concentration: 0.036
The calculated concentration has four significant figures, but it exceeds the maximum number
of decimal places. Therefore, the result is reported as 0.036 with three decimal places.
Note: This parameter has a Column Fill dialog that can be accessed by double-clicking on the
parameter's column header.
Max. Significant Figures: This column shows the maximum number of significant figures
that are displayed for the concentrations reported.
It is possible that the final result will not include the number of figures specified here,
depending on the value that is specified for Max. Decimal Places. See the examples under Max.
Decimal Places for more information.
Note: This parameter has a Column Fill dialog that can be accessed by double-clicking on the
parameter's column header.
You use this page to select various reporting options when using two or more wavelengths for
the same element. You can choose to:
• select the appropriate wavelength based on the concentration of the sample. You must
have a different concentration range for each wavelength. See the Select Line action
described below.
• report the average concentration of two or more wavelengths. You must have the
same concentration range for each wavelength. See the Average Lines or Report and
Average actions described below.
122 . Syngistix™ Software Guide
The list of analytes on this page is taken from the Method Editor Spectrometer: Define
Elements page, but only the analytes to which multiline calibration applies appear here. The
results will appear in the Results Display window.
Multiline Calibration: Select this check box to use multiline calibration.
Note: If the spreadsheet table is dimmed, you must select this check box to activate it.
Sequence: This column shows the order in which each analyte will be considered within each
element group. This is meaningful for only the Select Line action and can be changed using the
Move Up and Move Down buttons.
Element: This view-only column shows the elements in the current method that meet the
criteria for multiline calibration, that is, two or more wavelengths have been assigned to this
element. The elements are sorted first alphabetically and then by concentration range.
Action: This is how you want to have the concentration reported for each analyte.
Note: This parameter has a Column Fill dialog that can be accessed by double-clicking on the
parameter's column header.
used for this wavelength. Therefore, the Results Display window will show only the
result at Fe 234.349, 150 mg/L.
You can change the sequence using the Move Up and Move Down buttons. The
software will consider each wavelength in the sequence you specify.
Average Lines: Use this action to report an average concentration for an element at
two or more wavelengths. The concentration of an element is determined for each
wavelength. The three concentration values are averaged and the result is reported.
To use this action, you must have the same concentration range and units assigned to
each analyte. However, you can assign different calibration equations. One average
concentration per element can be calculated.
In the Results Display window, only the calculated average concentration is shown.
The average concentration is displayed with a new analyte name using the element
symbol and the word "Average." For example, "Ti Average."
Report & Average: Use this action to report individual concentrations for an element at
two or more wavelengths as well as the average concentration. In the example page shown
above, the concentration of zinc is determined for each wavelength, an average calculated
and all information reported. To use this action, you must have the same concentration
range and units assigned to each analyte. However, you can assign different calibration
equations. The Results Display window shows the concentration of the element at all
wavelengths and the calculated average of these concentrations.
Analytes: This view-only column shows all of the analytes in the current analysis that meet
criteria for multiline calibration. This information was entered on the Method Editor
Spectrometer: Define Elements page.
Low: This view-only column shows the lower limit of the calibration range. A zero appears
here for any calibration equation except linear or nonlinear bracketing. For either bracketing
equation, the lower limit that you entered in the Method Editor Calibration: Calibration Units
and Standard Concentration page will appear here.
High: This view-only column shows the upper limit of the calibration range. You entered this
information on the Method Editor Calibration: Calibration Units and Standard Concentration
page.
Units: This view-only column shows the units in which the concentration will be expressed.
Move Up (Button): When you choose Select Line, you use this button to move an analyte up
one place within the sequence of an element group. The software will consider each
wavelength in the sequence you specify.
Move Down (Button): When you choose Select Line, you use this button to move an analyte
down one place within the sequence of an element group. The software will consider each
wavelength in the sequence you specify.
124 . Syngistix™ Software Guide
Recalibration Page
You use this page to set up Recalibrations periodically during the analysis. You define the
calibration standards and blank solutions on the Define Standards Concentrations page.
Periodic Recalibrations
Select this check box to activate the recalibration options. The Periodic Recalibration
section is ignored if both of the following conditions are true:
• The Recalibrate Before parameter is active in the Sample Information File.
• Use sample info is checked in the Analysis window.
For both cases described above, the Sample Information setting overrides the Method Editor
setting.
Recalibration Type
Method checks are done in following cases:
• Reslope selected as the recalibration type, with no reslope defined in the method.
• Blank only selected as the recalibration type, with no calibration blank defined in the
method.
Complete Recalibration: The system analyzes the calibration blank(s) and all the calibration
standards, then creates a completely new calibration curve.
Reslope: The system analyzes the reslope standard, then calculates a correction factor and
uses it to change the slope of the active calibration curve .
Blank Only: The system analyzes the calibration blank and the reagent blank (if used) and
uses the new values for all subsequent sample analyses. The system does not change the
calibration curve. This compensates for changes in the zero absorption value since the
calibration curve was created.
126 . Syngistix™ Software Guide
Frequency
Every [n] samples: Select a value for [n]. The system performs a recalibration at regular
intervals, after analyzing [n] samples.
Note: QC's counted as samples will be part of the end sample count.
Checks P ages
Calculate Lim its Dialog
Use this dialog to calculate the upper and lower limits.
To display this dialog:
Click on the Calculate Limits... button on the QC Sample Concentrations and
Limits page of the Method Editor.
OR
Click on the Calculate Limits... button on the Sample Limits Checks page of the
Method Editor.
Using this dialog:
1. Specify the upper and lower limits in percent to be used to calculate the limits.
2. Click on OK.
Automatic limit calculation can only be done on a percentage basis of the entered
sample concentration. If you are accessing this dialog from the QC Sample
Concentrations and Limits page, please note that limits based on detection limits have
to be entered manually since the QC sample concentration is usually zero.
Recovery Checks
You use this page to enter the concentrations of analytes added to matrix recovery check (i.e.
"spike") samples analyzed using this method. Scheduling of matrix recovery check samples for
an analysis is performed using the Sample Information Editor.
Concentration Units
Calibration: Select this option to perform recovery calculations using the matrix check sample
concentrations expressed in Calib Units.
Sample: Select this option to perform recovery calculations using the matrix check
sample concentrations expressed in Sample UnitsAnalyte: This view-only column
shows all the analytes selected for the current analysis. To change the parameter, use the
entry field on the Spectrometer: Define Elements page.
Table
Conc Units: This view-only column shows Calibration Units or Sample Units, depending on the
selection made at the bottom of this page.
Recovery Set 1 to Set 6: These are the concentrations of analytes added to samples to
create matrix recovery check (i.e. "spike") samples to be analyzed using this method. You may
enter up to six different sets of concentrations for each method. In an analysis, a recovery set
can be used more than once. For example, you may analyze three recovery check samples that
are spiked with high analyte concentrations as defined in Set 1 and three other recovery check
samples that are spiked with low analyte concentrations as defined in Set 2.
To perform spike recovery measurements, you must enter information about the matrix check
samples in the Sample Information Editor using the Matrix Check Sample Entry dialog . The
equation used to calculate recovery checks is shown in the help topic for the Matrix Check
Sample Entry Dialog.
Note: This parameter has a Column Fill dialog that can be accessed by double-clicking on the
parameter's column header.
Note: The “If upper limit is exceeded, then dilute by [N] and reanalyze “check box only appears
when an ESI with prepFAST is installed and configured.
limits for the analytes where a concentration is specified. Or, you can simply enter a value in
the Upper and/or Lower Limit cells for a particular analyte.
If you have an ESI with prepFAST installed and configured you can also use this page to apply
a dilution if an upper sample limit check is exceeded.
To display the Sample Limits page:
1. Open the Method Editor.
2. Click on the Checks tab on the top of the Method Editor window.
3. Click on the Sample Limits tab page.
To automatically calculate limits:
1. Enter the sample Concentrations.
2. Click on the Calculate Limits... button.
The Calculate Limits dialog appears.
3. On the Calculate Limits dialog specify the upper and lower limits in percent to be
used to calculate the limits.
4. Click OK.
You are returned to the Sample Limits page and limits are only calculated for analytes
that have a Concentration specified.
5. Select whether you want concentrations expressed in Calibration units or Sample units.
6. Check the Show range along with limit remark option to have the range displayed
on the results screen along with the upper/lower limit fail message, if a sample falls
above/below the specified limit.
Note: Whenever you change the parameters on the Calculate Limits dialog and click OK, the Upper
and Lower Limits, displayed on the Sample Limits page, are automatically updated for all
analytes that have a concentration specified.
Note: To use this feature Concentration Units must be set to Calibration. Sample units cannot
be selected when "To apply a dilution if an upper sample limit check is exceeded" is checked.
130 . Syngistix™ Software Guide
Note: If a failure of a limit persists, the dilution action will only occur 3 times before continuing on to
the next sample.
4. In the example below, the upper limit for Zn is 0.5 mg/L. If this upper limit is
exceeded for any sample, then the sample will be re-run with a dilution factor of 10. If
the sample was originally run diluted, as specified in the Sample Information File, the
dilution value specified in this window will be applied as a multiplier.
Method Editor . 131
QC P ages
You use the QC pages to enter parameters that describe quality control samples. QC samples
are used to perform runtime checks of instrument performance. You schedule when and under
what conditions the QC samples are to be analyzed. QCs can be scheduled after the initial
calibration, after any recalibration, periodically throughout the analysis and at the end of the
analysis.
The periodic QCs also can be scheduled in the Sample Information Editor. If periodic QCs are
scheduled in both the Method Editor and the Sample Information Editor, then the Sample
Information Editor takes precedence.
To display the QC pages:
Click on the QC tab on the top of the Method Editor window.
To perform QC analyses:
To enter the required QC information, you must perform these steps:
1. Enter descriptive information about each QC sample including the QC sample ID and
autosampler ___location on the first QC page.
2. Enter the concentration and the upper and lower limits for each QC sample on the
second QC page. The software can calculate the upper and lower concentration limits,
or those limits can be entered manually.
3. Select when each QC sample is to be analyzed on the third QC page. The frequency
can be the same for all QC samples or different for each one.
Note: QC Samples can also be scheduled using the Sample Information Editor.
4. Select the action to be performed when the measured concentration is outside of the
acceptable limit for each QC sample on the fourth and fifth QC pages.
5. Select the maximum number of times a group of standards or standards and samples
may be reanalyzed to prevent the system from going into an infinite loop on the
Actions: End and Retry page.
QC Pages
Click on the appropriate tab on the right side of the Method Editor to select the pages.
QC Sample Definition Page
• QC Sample: Concentrations and Limits Page
• Schedule for QC Analyses Page
• Failure Actions for After-Calibration and Periodic QC's Page
• Failure Actions for At-End QC's
QC Sample ID: This is the quality control sample ID that will be displayed in the Results
Display window and in the results data set and printed or sent to a log file. You must first enter
an ID in order to enter any other information for a QC. The maximum number of characters is
20.
Autosampler Location: The software will automatically assign the next available
autosampler ___location when a QC Sample ID is entered. Enter the autosampler ___location for each
quality control sample if the ___location selected by the system is not appropriate.
Click on an entry field and type a value between 0 and the maximum ___location number
on your autosampler tray.
Count as Sample: If you want the QC to be considered part of the sample count, select this
box. For example, for a frequency of every 10 samples, there are nine unknown samples and
one QC sample.
Subtract Reagent Blank: Selecting this box for this parameter will cause the reagent blank
concentrations to be subtracted from the measured QC Sample concentrations.
If the QC Sample is to be analyzed as an unknown sample, then you would normally
subtract the reagent blank. If the QC Sample is a calibration standard that is similar in
matrix to the unknown sample and was reanalyzed to check the calibration, then you
would not subtract the reagent blank. This is because the reagent was not subtracted
from the calibration standard when the reagent was originally analyzed.
QC Sample ID: This specifies the QC sample whose parameters are displayed.
Analyte: This view-only column shows all the analytes selected for the current analysis. To
change the parameter, use the entry field on the Spectrometer: Define Elements page.
Units: This view-only column shows Calibration Units or Sample Units, depending on the
selection made at the bottom of this page.
Method Editor . 133
Concentration/Upper Limit/Lower Limit: This specifies the action limits for each QC
sample. If the measured concentration is between the specified upper and lower limits, no
action will be taken. If the measured concentration is above the upper limit or below the lower
limit, the appropriate failure action, which is defined on the appropriate Actions page, will be
performed.
To automatically calculate the upper and lower limits:
1. Enter the QC sample concentrations.
Since the significant figures and decimal places in the calculated limits are based on
those in concentration entries, you must enter the concentrations using enough
significant figures and decimal places so that the limits to be calculated have enough
significant figures and decimal places for proper limit checking. For example, if you
only use one figure for the concentration entry, then the limits will also have only one
figure.
2. Click on the Calculate Limits... button.
3. When the Calculate Limits dialog appears, specify the upper and lower limits in percent
to be used to calculate the limits.
4. Click on OK.
Automatic limit calculation can only be done on a percentage basis of the entered QC
sample concentration. Limits based on detection limits have to be entered manually
since the QC sample concentration is usually zero.
Note: This parameter has a Column Fill dialog that can be accessed by double-clicking on the
parameter's column header. You also enter the QC concentration for the analytes of interest.
Calculate Limits... This button displays the Calculate Limits dialog, which you use to
calculate the upper and lower limits for QC samples.
Schedule QCs
This page is used to enter the schedule for the QC analyses.
Note: QC samples can also be scheduled using the Sample Information Editor. If scheduling is done
using the Sample Information Editor, this takes precedence over any scheduling in the Method
Editor.
Note: If you schedule one or more After Initial Calib QC samples and then perform an Automated
Analysis using the Analyze Sam ples button, the instrument will analyze the QC as part of the
sample list. This is useful if you wish to use an existing calibration curve, analyze the After
Initial Calib QC sample as a check (without reanalyzing your calibration standards), then take
action based on the pass or fail status of the QC.
After Recalibration: The QC will be analyzed after any recalibrations that are part of the
analysis.
Periodically: The QC will be analyzed at specified intervals during the current analysis, based
on the frequency you select.
Frequency: This is the frequency at which the periodic QC samples are analyzed. For
example, if you select a frequency value of 20, then every 20 samples the QC sample will be
analyzed.
If you use the same frequency for all periodic QC samples, the values in the Frequency row in
the table will have a grey background and cannot be changed.
If you select Variable for the frequency, the values displayed in the table will have a white
background. You may then enter different frequency values for each QC sample.
At End: The QCs will be analyzed at the end of the current analysis.
continues. If all tries fail, the failure action will be performed. If you select None from the drop-
down list, the QC will not be reanalyzed. Instead, the system will go directly to performing the
failure action.
When All Tries Fail: Select a failure action from the drop-down list:
Note: If there are any after-calibration QCs, they will be analyzed after the recalibration action. If the
QCs pass, then the rest of the action is performed (continue or rerun samples).
Continue: The system prints a failure message and any optional message that you typed and
continues with the analysis.
Recal & Cont: The system prints a failure message and any optional message that you typed.
The system performs a complete recalibration as defined on the Calibration page including the
reagent blank if selected, then continues with the analysis.
Rslp & Cont: The system prints a failure message and any optional message that you typed.
The system analyzes the calibration blank and reslope standard as defined on the Calibration
page including the reagent blank if selected, then continues with the analysis.
AZ & Cont: The system prints a failure message and any optional message that you typed.
The system performs an autozero using the calibration blank and the reagent blank (if you are
using one), then continues with the analysis. An autozero sets the reading of the calibration
blank or reagent blank to zero automatically.
Alarm and Pause: The system prints a failure message and any optional message that you
typed. An alarm is activated and the analysis pauses. At this point, you will get an option to
stop or continue the analysis. If an automatic shutdown is scheduled, Alarm and Pause will
prevent system shutdown.
Next Method: The system prints a failure message and any optional message that you typed.
The current method is stopped and the system proceeds to the next method, if any. If there is
no next method, the system stops the analysis. If an automatic shutdown is scheduled, Next
Method will prevent system shutdown.
Stop: The system prints a failure message and any optional message that you typed. The
system stops the analysis. If an automatic shutdown is scheduled, Stop will prevent system
shutdown.
Additional Message: The system will automatically print standard messages indicating what
is happening if the measured QC concentration does not fall within the range specified by the
limits.
You can type an optional message up to 60 characters in length in this entry field that will be
printed when a failure action is performed in addition to the standard message.
Note: If there are any after-calibration QCs, they will be analyzed after the recalibration action. If the
QCs pass, then the rest of the action is performed (continue or rerun samples).
136 . Syngistix™ Software Guide
Continue: The system prints a failure message and any optional message that you typed and
continues with the analysis.
Recal & Cont: The system prints a failure message and any optional message that you typed.
The system performs a complete recalibration as defined on the Calibration page including the
reagent blank if selected, then continues with the analysis.
Rslp & Cont: The system prints a failure message and any optional message that you typed.
The system analyzes the calibration blank and reslope standard as defined on the Calibration
page including the reagent blank if selected, then continues with the analysis.
AZ & Cont: The system prints a failure message and any optional message that you typed.
The system performs an autozero using the calibration blank and the reagent blank if selected,
then continues with the analysis. An autozero sets the reading of the calibration blank or
reagent blank to zero automatically.
Alarm and Pause: The system prints a failure message and any optional message that you
typed. An alarm is activated and the analysis pauses. At this point, you will get an option to
stop or continue the analysis. If an automatic shutdown is scheduled, Alarm and Pause will
prevent system shutdown.
Recal & Rerun: The system prints a failure message and any optional message that you
typed. The system performs a complete recalibration as defined on the Calibration page
including the reagent blank if selected. Then, the samples are rerun, starting after the last QC
that passed.
Reslp & Rerun: The system prints a failure message and any optional message that you
typed. The system analyzes the calibration blank and reslope standard as defined on the
Calibration page including the reagent blank if selected. Then, the samples are rerun, starting
after the last QC that passed.
AZ and Rerun: The system prints a failure message and any optional message that you
typed. An autozero is performed using the calibration blank and the reagent blank if selected.
Then, the samples are rerun, starting after the last QC that passed. An autozero sets the
reading of the calibration blank or reagent blank to zero automatically.
Next Method: The system prints a failure message and any optional message that you typed.
The current method is stopped and the system proceeds to the next method, if any. If there is
not a next method, the system stops the analysis. If an automatic shutdown is scheduled, Next
Method will prevent system shutdown.
Stop: The system prints a failure message and any optional message that you typed. The
system stops the analysis. If an automatic shutdown is scheduled, Stop will prevent system
shutdown.
Additional Message: The system will automatically print standard messages indicating what
is happening if the measured QC concentration does not fall within the range specified by the
limits.
You can type an optional message in this entry field that will be printed when a failure action is
performed in addition to the standard message.
Note: If there are any after-calibration QCs, they will be analyzed after the recalibration action. If the
QCs pass, then the rest of the action is performed (continue or rerun samples).
Continue: The system prints a failure message and any optional message that you typed and
continues with the analysis.
Recal & Rerun: The system prints a failure message and any optional message that you
typed. The system performs a complete recalibration as defined on the Calibration page
including the reagent blank if selected. Then, the samples are rerun, starting after the last QC
that passed.
Rslp & Rerun: The system prints a failure message and any optional message that you typed.
The system analyzes the calibration blank and reslope standard as defined on the Calibration
page including the reagent blank if selected. Then, the samples are rerun, starting after the
last QC that passed.
AZ & Rerun: The system prints a failure message and any optional message that you typed.
An autozero is performed using the calibration blank and the reagent blank if selected. Then,
the samples are rerun, starting after the last QC that passed. An autozero sets the reading of
the calibration blank or reagent blank to zero automatically.
Alarm and Pause: The system prints a failure message and any optional message that you
typed. An alarm is activated and the analysis pauses. At this point, you will get an option to
stop or continue the analysis. If an automatic shutdown is scheduled, Alarm and Pause will
prevent system shutdown.
Next Method: The system prints a failure message and any optional message that you typed.
The current method is stopped and the system proceeds to the next method, if any. If there is
no next method, the system stops the analysis.
Stop: The system prints a failure message and any optional message that you typed. The
system stops the analysis. If an automatic shutdown is scheduled, Stop will prevent system
shutdown.
138 . Syngistix™ Software Guide
Additional Message: The system will automatically print standard messages indicating what
is happening if the measured QC concentration does not fall within the range specified by the
limits.
You can type an optional message up to 60 characters in length in this entry field that will be
printed when a failure action is performed in addition to the standard message.
Options Page
You use the entries on the Options page to set up your Results Display and Printed Log. You
also set some options for information to be stored with a Results Data Set for an analysis.
Display over calibration message: Select this option to display an over calibration message
when the sample concentration is greater than the entered percentage of the highest standard.
When this option is checked the % spin box is enabled. In the % spin box enter a value
between 100 and 999 %.
Note: For manual analyses, you must select the Calibration Summary command in the Analysis menu.
Detailed Cal. Summary: Select this option to display a detailed summary of each calibration
curve, including the calculated concentration of each standard. This summary will be displayed
after the final standard has been run.
Note: If you have a dual view method, then the Radial and Axial radio buttons will become enabled
when Universal Data Acquisition is checked. You can then select the Radial radio button to
collect Universal Data in radial viewing mode, or you can select the Axial radio button to collect
Universal Data in axial viewing mode.
Remarks: Use this entry field to type your comments regarding the method.
Method Editor . 141
Note: When Universal Data Acquisition mode is enabled all of the spectral data is recorded behind
the scenes and only the data for elements defined in your method are reported. If, at a later
time, you wish to determine additional elements or measure at alternative wavelengths, you
can select the UDA data from a results data set and reprocess the data with a method that
contains the elements you want to measure. For more information on reprocessing UDA data
see Reprocessing Universal Data.
Note: If you have a dual view method, then the Radial and Axial radio buttons will become enabled
when Universal Data Acquisition is checked. You can then select the Radial radio button to
collect Universal Data in radial viewing mode, or you can select the Axial radio button to collect
Universal Data in axial viewing mode.
Note: You cannot perform an analysis with a method that has all three of the following parameters
enabled: Spectral Profiling, High Resolution, and Universal Data Acquisition. At least one of
these parameters must be unchecked in order for your method to be valid. For example, you
can perform an analysis using a method that has Spectral Profiling and Universal Data
Acquisition enabled.
measure at alternate wavelengths. The steps outlined below show you how to reprocess UDA
data.
To reprocess UDA data:
1. On the Results tab in the Results group, click Reprocess.
The Data Reprocessing Window is displayed.
2. Next to Data Set to Reprocess, click on Browse... and select a results data set that
contains the data you want to reprocess.
Results data sets that contain Universal Data are marked with a > in the row number.
In the Data Reprocessing window, the results from the reprocessed data will be saved
to the data set shown in the Reprocessed Data Set field. This field defaults to the data
set from the most recent analysis. A check mark appears in the Save Reprocessed Data
box, confirming that reprocessed data will be saved. If you do not want to store
reprocessed data, uncheck Save Reprocessed Data.
3. To change to a different data set, click on Browse... (next to Reprocessed Data Set).
The Select Results Data Set dialog appears.
4. Type in a new data set name or select an existing one and then click OK.
5. Open the method that you want to use for reprocessing.
6. Confirm that the method in use contains the correct settings for the results data set
that is to be reprocessed.
7. In the Data Reprocessing table, review the information. The IDs in the selected
results data set are listed along with the sample information that was used when the
data was originally collected.
8. To edit this information, type the new information into the fields as desired. To access
a pop-up menu containing commands for editing the table, right click anywhere in the
table.
Note: There is a column fill dialog available for each of the parameters in the table, except Sample
Type and Original Method. To access a column fill dialog, double-click on the parameter's
column header.
9. To hide columns that do not contain data, check Hide Empty Columns.
Method Editor . 143
10. To only display samples with UDA data check Only show samples with Universal Data.
11. To select items of interest for reprocessing, select the associated row numbers in the
table.
12. To select a series of rows, click on the first row number of interest, hold down the Shift
key, and click on the last row number of interest. You can also drag over the row
numbers column using the mouse cursor.
13. To select non-consecutive rows, hold down the Ctrl key and click on each row
number.
Tip: The order in which samples are selected is the order in which reprocessing occurs. As you
select each row, the reprocessing sequence appears in the Sequence column.
File Form at
The sample information is written as a text file, a format that you can also create using other
software such as a BASIC program, a spreadsheet program, or a database program. You can
also create this file on a laboratory information management system and load it into your
instrument control computer to perform analyses.
Sample Information Editor . 147
Note: You can drag the mouse cursor through a range of samples in the Sample Information Editor
and, when you click on the Append to Analysis List button and the Append to Run List
dialog appears, the range of the selected samples already appears in the dialog.
2. Select a design from the list of Available Designs and click on OK.
This list includes a Default design and any other designs that have been previously
created and stored.
3. To create a name for the Sample Information File, in the Sample Information
group on the ribbon, click on the down button next to Save and select Save Design
As from the drop-down list.
4. You can customize the Sample Information Editor by selecting the parameters you
need to describe your samples. See Customizing the Sample Information Editor.
5. Enter the sample information.
For example, autosampler locations, Sample ID, Initial Sample Weight, etc.
6. If desired, annotate the file using the File Description field to provide further
descriptive information.
When you move the mouse cursor to this text area and click with the right mouse
button, a pop-up menu of editing commands appears.
7. Click on the down button next to Save and select Save Sample Information File
As from the drop-down list.
The Save As dialog appears. Type a name for the file, then click on Save.
Sample Information Editor . 149
Note: If this file has been modified but not saved, the file name in the dialog header will have an
asterisk ( * ) displayed to the right of the name. Once the file is saved, the asterisk will be
removed.
b. Select a Design from the list of Available Designs and click on OK. This list
includes a default design and any other designs that have been previously
created and stored. To create a name for the Sample Information File, in the
Sample Information group, click on Save As then in the Save Sample
Information As dialog type a name for the new sample information file, then
click on Save.
3. In the list of Available Parameters, click on a parameter to select it. (To deselect
the parameter, click again.) The parameters are shown in alphabetical order.
4. Click on the arrow button that points to the list where you wish to move the
selected parameter. Parameters marked with an asterisk (*) override settings in the
method.
150 . Syngistix™ Software Guide
• If the entry for the parameter is common to all samples, move the parameter to
the Common list.
• If the entry for the parameter varies for each sample, move the parameter to the
Variable list. For example, the analyst name might be the same for all samples,
while the sample IDs would vary for each sample. The parameter is removed
from the Available list and appears in the list you chose.
• To change your selections, click on a parameter in the Common list or in the
Variable list, then click on an arrow pointing back to the Available list. The
parameter is returned to the Available list.
5. Select additional parameters, if desired, and move them to the appropriate lists.
When you are finished, click on OK.
6. In the Sample Information Editor, use the scroll bars to see the changes you made.
Parameters that you added to the Common list appear in the Common
Parameters table, and those added to the Variable list appear in the Parameters
That Vary by Sample table.
Rem oving Param eters from the Sam ple I nform ation Editor
Click with the right mouse button anywhere on the background area in the Sample
Information Editor. In the pop-up that appears, select Parameter List... Click on a
parameter in the Variable list, then click on an arrow pointing back to the Available list.
To save the sample information design:
1. Click on the down button next to Save and select Save Design As from the drop-
down list. The Save Sample Information Design File As dialog appears.
2. Type a name for the file, then click on Save.
Note: If you modify a sample information file and then attempt to create a new one, a message
appears asking if you wish to save the changes to the first sample information file. This also
happens when you attempt to exit the Syngistix software.
2. Click with the right mouse button anywhere on the background area in the Sample
Information Editor. In the pop-up that appears, select Print.
3. In the Print dialog that appears, check that the correct printer is shown. To select a
different printer, click on the drop-down arrow in the Name field and make a selection.
To make other changes, such as paper size or graphic attributes, click on the
Properties button.
4. Click on OK to start printing.
Sample Information Editor . 153
Note: When you clear information, the content in an entry field is removed, not the entry field itself.
1. Click on the entry field that contains the information you want to remove.
2. On the Analysis tab, in the Edit group, click on Clear.
- or -
Click with the right mouse button. A pop-up menu appears. Click on Clear.
- or -
Press the Delete (Del) key.
Note: When you insert rows, the new rows are inserted before the first row you select in the table.
1. Select a row in the table by clicking on a number in the Sample Number column of
the table. The entry fields in the row become highlighted to indicate that the row is
selected.
2. If you want to insert more than one row, you select the same number of rows in the
table. For example, to insert three new rows, you would select three existing rows.
To select additional rows, hold down the Shift key while clicking on additional row
numbers.
3. On the Analysis tab, in the Edit group, click on Insert Rows.
- or -
Click with the right mouse button. A pop-up menu appears. Click on Insert Row.
To summarize, for the above example, you would enter the following values:
Aliquot Volume 10 mL
Note: You can also record the Diluted to Volume as the ratio of the original sample volume to the
final sample volume. In this example, 10 mL of sample is diluted to 100 mL, so the ratio
would be 10:100 or 1:10. You can enter 1 for Aliquot Volume and 10 for Diluted to Volume.
Sample Information Editor . 157
3. In the Available list, click Auto Dil. Factor#. (To deselect the parameter, click
again.)
4. Click on the arrow button that points to the Variable list.
The Auto Dil. Factor# is moved to the Variable list.
5. Click OK to close the Sample Information Parameters dialog.
The Auto Dil. Factor# parameter now appears in the Parameters That Vary By
Sample list on the Sample Information Editor.
158 . Syngistix™ Software Guide
Sam ple ID
This is the name you give to each sample.
• Type up to 25 characters for each sample. You can use any combination of letters
and numbers.
- or -
• To automatically enter a sequence of IDs, double-click on an entry field and use the
Sample ID Column Fill dialog.
Rem ark s
Click on the entry field. The Remarks Entry dialog appears, in which you can type up to 50
characters.
Analyst Nam e
This is the name of the person setting up or performing the analysis.
• Type up to 20 characters for each sample. You can use any combination of letters
and numbers.
- or -
• To automatically enter a sequence of names, double-click on an entry field and use
the Column Fill dialog. Note: If the name is the same for all samples, assign this
parameter to the Parameters Common to All Samples table.
162 . Syngistix™ Software Guide
User Defined...
Use this parameter to define your own parameter. For example, you may want to record an
account name for the batch of samples. You can customize up to five sample information
parameters. Select User Defined... in the list of parameters, then type a name for the
parameter using up to 20 characters in the User Defined Entry field dialog.
If your And your Initial Sample Weight Initial Sample Vol. Aliquot Volume and
Calibration Sample and Sample Prep Vol. and Sample Prep Vol. Diluted to Volume.
Units are... Units are...
Optional
Wt/Vol Wt/Wt Required *
(but must enter both)
Optional
Wt/Vol Wt/Vol Enter both or omit both*
(but must enter both)
Optional
Wt/Wt Wt/Wt Not used in conversion Not used in conversion
(but must enter both)
The software will not convert Wt/Wt calibration units to Wt/Vol sample units. The
Wt/Wt Wt/Vol software will only report the sample concentration in calibration units, not sample
units.
N otes:
* Without the required entries, the software will only report the sample concentration in
calibration units, not sample units. If both entries are required and you only enter one, again,
the concentration in sample units will not be reported.
If you enter the Aliquot Volume, you must also enter the Diluted to Volume for correct
reporting of results.
You select calibration units and sample units in the Method Editor on the Calibration Units and
Concentrations page. Or, you can select sample units in the Sample Information Editor. If the
sample units in the Sample Information Editor differ from those in the Method Editor, the
sample units in the Sample Information Editor will be used.
Sample Preparation Parameters: The Sample Preparation parameters are shown below.
For an example using Initial Sample Weight, Sample Prep Volume, Aliquot Volume, and
Diluted to Volume see, Sample Preparation: An Example.
Aliquot Volume: If an aliquot of the sample solution is taken and diluted to a final volume,
record the aliquot volume for this entry and the final volume for the Diluted to Volume entry.
Enter the volume using the units selected for the Volume Units. To automatically enter the
same value for a sequence of samples, double-click on an entry field and use the Aliquot
Volume Column Fill dialog.
Diluted to Volume: This is the final volume of solution obtained by diluting an aliquot of
the sample solution.
You can also record the dilution as the ratio of the original sample volume to the final sample
volume. For example, if 10 mL of sample is diluted to 200 mL, this ratio would be 10:200 or
1:20. Enter 20 for the Diluted to Volume entry and 1 for the Aliquot volume. Enter the
volume using the units selected for the Volume Units. To automatically enter the same value
for a sequence of samples, double-click on an entry field and use the Diluted to Volume
Column Fill dialog.
Sample Information Editor . 163
Solids Ratio: This is the ratio of the wet and dry weights for the sample. This ratio is used
to correct the sample concentration. For more information, see the Solids Ratio Column Fill
dialog.
Initial Sample Weight: If you weigh the sample during sample preparation, you must
enter the Initial Sample Weight and the Sample Prep Volume.
Enter the weight using the units selected for the Weight Units. To automatically enter the
same value for a sequence of samples, double-click on an entry field and use the Initial
Sample Weight Column Fill dialog.
Initial Sample Volume: If you measure the sample volumetrically during sample
preparation, you can enter the Initial Sample Volume and the Sample Prep Volume.
Enter the volume using the units selected for the Volume Units. To automatically enter the
same value for a sequence of samples, double-click on an entry field and use the Initial
Sample Volume Column Fill dialog.
Weight Units: Select the units for the weight value(s) you enter for each individual sample
or for all samples. These weight units are used for the Initial Sample Weight and the Nominal
Sample Weight entries. To automatically enter the same value for a sequence of samples,
double-click on the column header and use the Units Column Fill dialog.
Volume Units: Select the units for the volumes you enter for each individual sample or for
all samples. These weight units are used for the Initial Sample Volume, the Sample Prep
Volume, the Aliquot Volume, and the Diluted to Volume entries. To automatically enter the
same value for a sequence of samples, double-click on the column header and use the Units
Column Fill dialog.
Sample Prep Volume: After a solid sample has been dissolved or a liquid sample has been
acidified (or otherwise treated), the resulting solution is prepared to a specific volume. This is
the Sample Prep Volume. Enter the volume using the units selected for the Volume Units. To
automatically enter the same value for a sequence of samples, double-click on an entry field
and use the Column Fill dialog.
Nominal Sample Weight: This is the target weight when samples are weighed. This entry
is required only if corrections are being made to weight/volume measurements to
compensate for weight variations among samples. The Nominal Sample Weight is divided by
the Initial Sample Weight to correct the final concentration value. Enter the weight using the
units selected for the Weight Units. To automatically enter the same value for a sequence of
samples, double-click on an entry field and use the Column Fill dialog.
Sample Units: These are the units used to report the concentrations of the samples. If the
sample units in the Sample Information Editor differ from those in the Method Editor, the
sample units in the Sample Information Editor will be used. You can select different sample
units for different samples in the Sample Information Editor, but concentrations for all
elements will be reported using the same units. To automatically enter the same value for a
sequence of samples, double-click on the column header and use the Sample Units Column
Fill dialog.
Sample Limits: This parameter can be used to enable sample limit checks as defined in the
method. When this parameter is unchecked sample limit checks will not be performed on the
specific sample/s, although the active Method has Sample Limits enabled.
To select your own units:
The units available in the drop-down lists are stored in an ASCII file called UNITS.INIX
located in C:\Users\Public\PerkinElmer Syngistix\ICP\SystemFiles\Configuration. You can use
any text editor to add units to the file. You may also rearrange the units in the file so that
those used frequently are near the top of the list.
164 . Syngistix™ Software Guide
Note: Periodic QC Scheduling in the sample information file will override Periodic QC Scheduling in
the Method Editor.
Read Delay
Use this parameter to use a Read Delay that differs from the read delay that is entered in the
method. Enter the Read Delay in seconds. To automatically enter the same value for a
sequence of samples, double-click on the column header and use the Column Fill dialog.
Sample Information Editor . 165
W ash Tim e
Use this parameter to use a Wash Time that differs from the Wash Time that is entered in
the method. Enter the Wash Time in seconds. To automatically enter the same value for a
sequence of samples, double-click on the column header and use the Column Fill dialog. Note
that the Wash Frequency is selected in the method. You must select Between Samples for
the Wash Frequency in order for a wash to occur.
3. Select additional parameters, if desired, and move them to the appropriate lists.
When you are finished, click on OK.
In the Sample Information Editor, use the scroll bars to see the changes you made. Parameters
that you added to the Common list appear in the Common Parameters table, and those
added to the Variable list appear in the Parameters that Vary by Sample table.
To specify the maximum number of samples:
Use the up or down arrows to specify the number of samples you have and then
click on OK. In the Sample Information Editor, the Parameters that Vary by Sample
table will contain this number of rows, one for each sample.
Click on the first row in the range of samples and drag the mouse cursor over the
entry fields that you want to fill in the column. The rows are highlighted. Right click
then click on Column Fill...
Click on the first row in the range of samples and drag the mouse cursor over the
entry fields that you want to fill in the column. The rows are highlighted. Right click
then, click on Column Fill...
When you include the Recalibrate Before parameter in the SIF, a new Reagent Blanks
choice is added to the Calibration type drop-down list.
• If the Reagent Blanks option is selected for a sample, all reagent blanks required
by this sample are run immediately prior to the sample run (forced rerun of relevant
reagent blanks).
• Default operation is used in the following scenarios:
o The Reagent Blanks option is not selected.
o The Recalibrate Before parameter is not included at all.
• If a required Recalibrate Before has already been run since the last calibration, it
shall not be rerun (no forced rerun).
• If there is a reagent blank defined in the SIF but not in the method, this will trigger
an error dialog telling you this during Check Analysis.
To automatically enter recalibration information for a range of samples:
1. Select a recalibration, reslope, or autozero before the solution identified in this row is
analyzed. Select None or leave the entry field blank if you do not want any of these
options performed.
2. Select the frequency in which you want to recalibrate, then select the sample numbers
for a range of samples. For example, to recalibrate before every five samples in a range
numbered 10 through 20, select Schedule after every 5 samples, then select 10 for
the Start number and 20 for the End number. In this example, the software would
automatically recalibrate before Sample Numbers 15 and 20.
Additional considerations:
• When “Insert Sample” is used to add a priority sample during an analysis, the new
SIF fields are available as defined in the SIF.
You should set the appropriate fields at that time.
• A new check is added to “Check Analysis” such that all reagent blanks specified for
subtraction for any sample in the SIF are defined in the method.
• Reagent blanks specified during “Insert Sample” are already defined in the method
as part of the “Check Analysis” done when a sample is inserted.
New reagent blanks cannot be added.
The Reagent Blank Usage parameter defines reagent blank usage options for each sample
with options as follows:
• Average All. Subtract average of all reagent blanks defined in the method (default
operation).
• None. No reagent blank subtraction for this sample.
• Custom. Subtract the specified reagent blank (number 1-5), corresponding to
reagent blank numbers in the method. Enter a list of one or more reagent blank
numbers (1-5) separated by commas. Each specified reagent blank number must be
defined in the method used for analysis.
You set your options used for a range of samples in the Reagent Blanks Used Column
Fill dialog, which (as with other SIF parameters) is available in the following ways: Double-
clicking the field, where the dialog shall be used to make the selection for an individual
sample, or double-clicking the column header (the “column fill” dialog).
If desired, you can pre-select the range of samples in the Sample Information Editor by
selecting a range of entry fields in the column. When the dialog is displayed, this range will
automatically be entered.
• Click on the first row in the range of samples and drag the mouse cursor over the
entry fields that you want to fill in the column. The rows are highlighted. Right click
then click on Column Fill...
If you are analyzing a dry sample and want the result converted to a wet basis,
176 . Syngistix™ Software Guide
- or -
If you are analyzing a wet sample and want the result converted to a dry basis,
enter the ratio of wet weight divided by dry weight.
In either case, the concentration in calibration units is multiplied by the solids ratio
as part of the conversion from concentration in calibration units to concentration in
sample units.
2. Select the sample number range for your group of samples:
In the Start box, select the sample number for the first sample in the group.
In the End box, select the sample number for the last sample in the group.
3. Click on OK. The software enters the values in the Sample Information Editor.
To convert a measured concentration in calibration units to a final concentration in sample
units:
Duplicate
A matrix check duplicate measurement is performed. The software calculates the relative
percent difference using the equation:
where:
conc #1 = the result obtained for the concentration of the reference sample
conc #2 = the result obtained for the concentration of the duplicate sample
where:
conc #1 = the result obtained for the concentration of the reference sample
conc #2 = the result obtained for the concentration of the recovery sample
Diluted x fold
A matrix check dilution measurement is performed. Enter the dilution factor. This is the ratio
of the original sample volume to the final sample volume. For example, if 1 mL of sample is
diluted to 10 mL, type 10. The software calculates the percent difference using the equation:
Sample Information Editor . 179
where:
conc #1 = the result obtained for the concentration of the reference sample
conc #2 = the result obtained for the concentration of the diluted sample DF = dilution
factor
1. Select the sample number of the Reference Sample. This is the first sample in the
pair of matrix check samples. This sample must be scheduled for analysis before the
second sample in the pair.
2. Check the sample number for the Current Sample. Change the number, if necessary,
so that it is the matrix check sample, which is the second sample in the pair.
Analysis Control W indow
182 . Syngistix™ Software Guide
Note: In the Transient technique, the R ead Delay (sec) and the Override M ethod functions
are not applicable.
Analyze Standard
Click on this button to analyze the calibration standard shown in the entry field. The
results of this analysis are used to set up a calibration. To interrupt the standard
analysis, click again on Analyze Standard.
To change the standard shown in the entry field, select an option from the drop-
down list. The list shows all of the standards, including reslope, that you defined in
the active method. A calibration curve is created after all blanks and standards
defined in the method are run. To view a calibration curve, click on the Calib button,
or from the Options menu, click on Calibration Display.
184 . Syngistix™ Software Guide
To check the concentration values that were entered for the standard in the method,
click the Conc...button. In the View Standard Concentrations dialog that appears, the
concentrations and units of each standard are shown. To change the concentration of a
standard, use the Method Editor-Calibration-Calib Units and Concentration.
Analyze QC
Click on this button to analyze the Quality Control sample in the entry field. To
interrupt the standard analysis, click again on Analyze QC.
To change the standard shown in the entry field, select an option from the drop-
down list. The list shows the QC samples currently defined in method.
Note: When QC Samples are run from the Manual Analysis window the following information is
used from the active method: QC Sample ID, Count as Sample, Subtract Reagent Blank, the
content from the Concentrations and Limits tab page. Information defined on the Schedule
QCs tab and both Action tab pages of the Method Editor are ignored for QCs run in Manual
Mode.
Go to A/ S Loc.
Click on this button to move the autosampler probe to the selected autosampler
___location shown in the entry field. The Status Panel reflects this change.
Go to W ash
Click on this button to move the autosampler probe to the wash ___location. The
Autosampler Monitor reflects the change.
Override M ethod
When using the Read Delay process, this check box controls whether the instrument will use
the values in the active method or the changes you make in this window. If it is left blank,
the values in the active method are used. If the Override Method box is checked, the values
entered in this page are used. The values entered in the method are not changed.
Note: Override Method is not applicable in the Transient technique. Use Sample Info.
Analysis Control Window . 185
Note: The sample information file should contain entries for samples only. All other solutions, such
as blanks and standards, are defined in the Method Editor.
Note: For information on the amount of disk storage space that is required for your results, see
Equation for Calculating Disk Storage for Results.
Run List
The Run List on the right half of the window displays the corresponding sample information
and order in which they will be run.
Clear List: To clear the display click on this button.
Print List: To print the sequence, ___location, sample type, ID, and status information
shown, click on this button. The printed report also shows the current date and time as
well as the method name.
186 . Syngistix™ Software Guide
Insert Sample: To insert a new sample into the sequence (only during an analysis),
click on this button and in the Insert Sample dialog that appears, enter new sample
information.
Load Tray: Click on this button to raise the autosampler probe and move it to the back
so that the sample tray can be removed or installed. Click on Load Tray again to restore
the probe to its operating position.
You use this screen to select Methods and a Sample Information File. You also can select a
results data set to store the data, print an analysis log, and select other actions to occur
during an analysis.
Note: You can change setup options even after an analysis has begun by returning to this window.
Analytical Sequence dialog appears so that you can select the point where the interrupted
analysis will restart.
Calibrate
Click on this button to start the calibration sequence. The system uses the blank and
standards defined in the method.
To interrupt the calibration sequence, click again on Calibrate. The Stopping an
Analytical Sequence dialog appears so that you can select when the blank and
standard analysis will stop. If you stopped the blank and standard analysis, (and you
did not click on Reset Sequence), you may resume at a particular place in the
calibration sequence by clicking again on Calibrate. The Continuing an Analytical
Sequence dialog appears so that you can select the point where the interrupted
analysis will restart.
When calibration is complete, you may want to examine the calibration curves in the
Calibration window before analyzing samples.
Note: If you schedule one or more After Initial Calib QC samples in the method, Analyze
Sam ples will analyze the QC as part of the sample list. This is useful if you wish to use an
existing calibration curve, analyze the After Initial Calib QC sample as a check (without
reanalyzing your calibration standards), then take action based on the pass or fail status of
the QC. For more information on QCs see the Method Editor: QC Pages.
Note: If you have multiple methods, only the current method is rerun.
190 . Syngistix™ Software Guide
6. Click on OK. The system continues the analysis, based on the option selected.
Or, if you decide not to continue the analysis, click on Cancel.
Reset Sequence
This button resets the analytical sequence back to the beginning.
Click on this button to reset the analytical sequence to 1. The next time you click on
Analyze All, Analyze Samples or Calibrate, the sequence will be rebuilt and the
system will start with the first item in the list.
M ethod Source
Choose Use the Active Method for your Analysis which uses the active method
already in memory to analyze samples. (This is the normal choice when using a
single method to analyze samples.)
- or -
Choose Specify methods for your analysis which opens methods in the list to
analyze samples. (Use this option when you want to analyze samples using several
methods in a sequence.)
Method: You use this entry field to select the method(s) for the Automated analysis.
• Double-click on an entry field in the Method column. In the Open
Method dialog that appears, select a method.
Note: To select more than one method, you must first select the Method
source. This option is located below the Methods and Sample Locations table.
You can select up to 50 methods.
Delay (min): This is the time, in minutes, that the system waits before it starts the method.
(Maximum of 99 minutes)
Define By selecting samples from a sample information file, information you have
Samples: supplied about the samples (for example, sample weights or dilutions) is used
in the analysis. Use this column to specify the samples you want to use from a
sample information file.
First, open a sample information file. Then, select the check box for Use
Sample Info below the name of the sample information file. Then three
options appear in the Sample Info File column in a drop-down list. If you want
to analyze all of the samples in the sample information file, select All Defined
from the drop-down list. If you want to select only certain autosampler
locations, select Locations. If you want to select samples by the sample
numbers listed in the sample information file, select Sample Nos.
Locations: If you do not want to analyze all of the samples in the sample information file,
use this entry field to select only the autosampler locations of the samples that
you want to analyze. If you have selected All Defined or Sample Nos. in the
Sample Info File drop-down list, you cannot enter locations here. If you have
not selected the check box for Use Sample Information below the name of the
sample information file, the locations do not apply to a sample information file.
• Type individual locations or a range of locations. Use commas to separate
the locations and ranges. It is not necessary to enter the locations of
blanks, QC's, check or calibration solutions. Enter locations for these if you
want them to be treated as a sample within the analysis. Example: 10-
15, 18, 20, 22, 25-30.
Analysis Control Window . 191
Sample Nos: If you do not want to analyze all the samples in the sample information file,
use this entry field to select only the sample numbers that you want to
analyze. If you have selected All Defined or Locations from the Sample Info
File drop-down list, you cannot enter sample numbers here.
Example: If you only want to analyze #s 1, 3, 4, and 5, but not #2, in the
Sample Info File column, select Sample Nos. This opens the Sample numbers
field so that the sample numbers can be entered.
Append Method: This button is only enabled during an analysis. Click on this button to
display the Append Method dialog from where you can add methods to the run list after an
analysis has started.
Note: If a sample information file is not entered, the "Untitled" sample information file that is
currently open in the editor is listed.
Note: For information on the amount of disk storage space that is required for your results, see
Equation for Calculating Disk Storage for Results.
Note: You must first create the Export Design(s) in the Data Manager. An export design efines a
subset of data items that you want to export from a data set. For more information, refer to
Data Manager Help. When exporting data, you have the ability to select two of your designs
as Export Design 1 and Export Design 2. You may want to do this if you want different
information to be exported or you want the data to be exported to two separate file
locations. Remember, in each Export Design created you assign the directory path where you
want your results stored.
1. Click the check box for Export Design 1. The Open dialog appears.
2. Navigate to your desired Export Design (*.xptx) file.
3. If a file is displayed in the entry field, type the name of the design you created in the
Data Manager or click the open file browse button to the right of the entry field;
when the Open dialog appears select the name of the design (*.xptx) and click on OK.
4. If you want to export Particle Counter data, select Export Design 2.
5. Navigate to your desired Particle Export Design (*.pxpx) file.
6. If a file is displayed in the entry field, type the name of the design you created in the
Data Manager or click the open file browse button to the right of the entry field;
when the Open dialog appears select the name of the design (*.pxpx) and click on OK.
7. Click on OK.
A check mark appears in the Auto Export check box indicating that for each analysis
you perform, data will be exported automatically. To stop exporting data in this
manner, click on the check box to clear the check mark.
Scheduler
Click the Settings button to display the Automatic Shutdown/Startup dialog.
To schedule an automatic shutdown or Startup, click on Shutdown or Start-up. Select
options controlling time of and events to occur at shutdown and startup. This feature allows
you to shut down the plasma at the end of the analysis and start it up again at a later
specified time.
Note: The Auto W avelength R ealign option is not applicable in the Transient technique.
If more than one method is listed, you can view which method is being used for the current
analysis. The methods are numbered, type in, or click the arrow, to choose the Method
number.
Run List
The Run List on the right half of the window displays the samples associated with the
method and order in which they will be run.
Rebuild List: To refresh the display (to show changes you have made to the method or
sample information file), click on this button.
Print List: To print the sequence, ___location, sample type, ID, and status information
shown, click on this button. The printed report also shows the current date and time as
well as the method name.
Insert Sample: To insert a new sample into the sequence (only during an analysis),
click on this button and in the Insert Sample dialog that appears, enter new sample
information.
Load Tray: Click on this button to raise the autosampler probe and move it to the back
so that the sample tray can be removed or installed. Click on Load Tray again to restore
the probe to its operating position.
Note: The Enabled parameter has a column fill dialog that can be accessed by double-clicking on
the column header.
2. Click on OK.
Note: Analytes will remain disabled until re-enabled using this dialog or until a new method is
loaded.
Analysis Control Window . 195
Make the appropriate entries on the Set Up page of the Automated Analysis
Control window and then click on the Analyze tab.
In the Analysis group click on Autosampler Load List.
An example of an Autosampler Loading List window displays:
Note: In the list of autosampler Locations and Solutions, the method is not shown for samples
(unknowns).
Note: If a change is made to the method, SIF, or Auto Analysis window which affects the contents
of the Loading List, the Loading List window is automatically updated.
5. To print the list, right-click and then click on Print Autosampler Loading List or
click on the button and select Print Active Window. In the print dialog that
appears, select your printer and click on OK.
196 . Syngistix™ Software Guide
Note: Reprocess cannot be accessed unless the Analysis Control Windows are closed.
2. Next to Data Set to Reprocess, click the browse icon and select a results data set
that contains the data you want to reprocess.
3. In the Data Reprocessing window, the results from the reprocessed data will be
saved to the data set shown in the entry field. This field defaults to the data set from
the most recent analysis.
To change to a different data set, click the browse icon and in the Select Results
Data Set dialog that appears, type a new data set name or select an existing one.
4. The Method should be open in the Method Editor so if you want to reprocess using
different method parameters, that information can be used. Confirm that the method
in use contains the correct settings for the results data set that is to be reprocessed.
5. In the Data Reprocessing dialog table, review the information. The IDs in the
selected results data set are listed along with the sample information that was used
when the data was originally collected. To edit this information, type the new
information into the fields as desired. To access a pop-up menu containing
commands for editing the table, right click anywhere in the table. To hide columns
that do not contain data, select the Hide Empty Columns check box.
Note: There is a column fill dialog available for each of the parameters in the table, except Sample
Type and Original Method. To access a column fill dialog, double-click on the parameter's
column header.
To select items of interest for reprocessing, select the associated row numbers in the
table. To select a series of rows, click on the first row number of interest, hold down
the Shift key, and click on the last row number of interest. You can also drag over
the row numbers column using the mouse cursor. To select non-consecutive rows,
hold down the Ctrl key and click on each row number.
Tip: The order in which samples are selected is the order in which reprocessing occurs. As you
select each row, the reprocessing sequence appears in the Sequence column.
6. Click on Reprocess.
header and the data that is shown in the Results Display window as selected on the Options
page of the Method. Look at all of the selections on the Method Editor Window Options page
to get an overview of the selected analytical results that will appear in the printout.
Hide Empty Columns: Select this box to hide columns that do not contain data.
Only show samples with Universal Data: Select this box to filter the display so that only
samples that were collected with the Universal Data Acquisition parameter enabled in the
method are displayed.
Select all samples in current order: Checking this box selects all samples in the order
they are displayed when you open a data set.
Number of samples selected: Displays the number of samples selected for reprocess.
Note: For an example using Initial Sample Weight, Sample Prep Volume, Aliquot Volume, and
Diluted to Volume see, Sample Preparation: An Example.
Sequence: This is the sequence in which samples will be reprocessed. This sequence
appears as you select each row number.
Sample ID: This is the name you gave to each sample.
Sample Type: This is the solution type: blank, standard, sample, etc.
Omit Replicates: This is the entry for replicate numbers that you do not wish to reprocess
for a sample.
Matrix Check Samples: This shows any samples that are designated as matrix checks.
Date/Time: This shows the date and time that each sample was analyzed.
Initial Sample Wt: This is the quantity of sample weight before sample preparation.
Initial Sample Vol: This is the quantity of sample volume before sample preparation.
Sample Units: Use this column to change the sample units on a per sample basis before
reprocessing data. The concentration will be calculated based on the new units. (All of the
analytes in a sample must have the same sample units to use this parameter.)
Weight Units: This shows the units of the Initial Sample Quantity. These are either weight
or volume units.
Sample Prep. Volume: After a solid sample has been dissolved or a liquid sample has been
acidified (or otherwise treated), the resulting solution is prepared to a specific volume. This is
the Sample Prep Volume.
Aliquot Volume: If an aliquot of the sample solution is taken and diluted to a final volume,
record the aliquot volume for this entry and the final volume for the Diluted to Volume entry.
Diluted to Volume: This is the final volume of solution obtained by diluting an aliquot of
the sample solution. You can also record the dilution as the ratio of the original sample
volume to the final sample volume. For example, if 10 mL of sample is diluted to 200 mL, this
ratio would be 10:200 or 1:20. Enter 20 for the Diluted to Volume entry and 1 for the Aliquot
volume.
Volume Units: If the final sample concentrations are being reported in weight/weight units,
you must enter the units for the Sample Volume.
Solids Ratio: This is the ratio of the wet and dry weights for the sample. This ratio is used
to correct the sample concentration. For more information, see the Solids Ratio Column Fill
dialog.
Nominal Sample Weight: This is the target weight when samples are weighed. This entry
is required only if corrections are being made to weight/volume measurements to
Analysis Control Window . 199
compensate for weight variations among samples. The Nominal Sample Weight is divided by
the Initial Sample Weight to correct the final concentration value.
Batch ID: This is the name you give to this batch of samples.
Original Method: This shows the method you used in the analysis. This information cannot
be modified.
Remarks: The remarks you entered in the Sample Information file before the initial analysis.
Sample Limits: Check this box to enable sample limit checks as defined in the method. If
you uncheck this parameter, then sample limit checks will not be performed for the particular
sample.
200 . Syngistix™ Software Guide
Samples = actual samples + no. of standard analyses + no. of blank analyses + no. of QC
analyses (i.e. number of entries in analysis list)
Type-factor =
When you initially start a new software session, or after you click Clear Data, the Data Viewer
tabs are empty. They become populated as data is acquired, regardless of whether or not the
window is open in your workspace. As you run samples, the tabs are updated in real time. The
table-based tabs collect a scrolling list of sample results collected during quantitative analyses
to a maximum of 1000 samples, after which the first samples scroll off the top of the list as
new samples continue to be added at the bottom. Index numbering of the developing list goes
up to a maximum count of 9,999 before rolling over to begin at 1 again.
To help you keep track of where you are in the data, your position in the scrolling list on any
table is retained when you move between the Corrected Intensities, Conc. in Calib Units, and
Conc. in Sample Units tabs, so that you can compare multiple types of data for a single
sample without losing your place. In addition, the calibration curves are displayed in-line in
the table.
In the tables, sample data is displayed in alternating rows of white and gray to improve
readability. Additional color cues employed in the tables include the use of a red font to
indicate QC failures, and the standard KED mode green and DRC mode yellow used in the
column headers to indicate analytes using these modes. On the Conc. tab, a purple font is used
to denote internal standards, which are also identified with an (IS) in the relevant analyte
header. Note that all tables take their base colors from your system colors; if you change from
the default Windows system colors, you may change the table background colors.
Data Viewer . 203
Note: If a QC measure specifies that there be a valid calibration in the current workspace, and
none exists, the QC Status column will appear blank, rather than showing P assed or Failed.
The QC status will also be blank if QC checking is not enabled in the given method; or when
it is enabled, but no QC limits have been specified.
206 . Syngistix™ Software Guide
Note: The internal standards calculations performed on this tab are completely independent of
those performed through the QC functions; activation of QC checking in the method is not
required for the plotting of internal standards data on this tab.
When a value is in shutdown, an S appears at the top of the graph, with the plot lines
extending up outside of the top boundaries of the graph on either side. See Reported
Shutdown for more information.
When you move your mouse over a point in the graph a screen tip appears displaying the
following additional information for that point: row index and sample ID numbers; analyte
name and mass; % recovery; intensity; and units used for the intensity.
Blanks and normalization factors
On the Report window Internal Standards tab, the internal standards plotted are normalized
against the most recent blank processed, for all samples, and across multiple methods, until
a new blank is introduced. Each blank effects a new normalization factor specifically and only
for those internal standards listed in that blank, cancelling all previous factors for all
subsequent internal standards.
If a blank is not present, or no internal standards are defined in the blank, then a
normalization factor cannot be defined, and no internal standards points are plotted on the
graph. Other situations in which normalization cannot be factored include cases in which the
intensity of an internal standard in the blank is zero, or where the internal standard is in
shutdown, or is in brackets (wherein one of its equation analytes is in shutdown).
In addition, all existing normalization factors are cleared if you manually clear the current
Blank or Calibration & Blank via the Analysis menu. Also, if you open or create a new
calibration file, load a calibration in the Dataset window, or run an operation that loads a new
calibration file (such as reprocessing a blank, standard, or sample using original conditions),
the normalization factors will again be cleared.
When the normalization factor is undefined or has been cleared, no points are plotted on the
graph until a new, valid blank is run and normalization is re-established. In the case of
reprocessing, no points are plotted as long as the Use Original Conditions check box is
selected, as sufficient data is not available.
Note: Where only a single blank has been run, no point is plotted on the graph; plotting begins at
the next sample. Also, when a new blank is run, no point is plotted on the graph for the
blank; plotting resumes immediately thereafter.
208 . Syngistix™ Software Guide
QC Tab
This tab displays relevant Quality Control data for samples run for which QC criteria has been
defined in the selected method. The data displayed includes the basic sample information, such as
the originating row index number and analyte sample information. Analytes that are acting as
Internal Standards are identified with an (IS) in the relevant analyte header. When a sample falls
outside of the specified QC criteria, the relevant data is displayed in red text. QC data is displayed
for only as long as the corresponding sample entries appear on the Intensities, Concentrations, and
Unfactored Concentrations tabs.
The data on the QC tab is organized into the following categories: QC Standards; QC Spikes;
QC Duplicates; QC Dilutions; and Samples, Blanks, and Calibration Standards:
• For QC Standards, which are grouped by standard number, the original sample concentration is
displayed, followed by the RSD and % recovery.
• QC Spikes display the % recovery of the spike. QC Duplicate Spikes are also listed here, showing
the % difference. For all QC Spikes and QC Duplicate Spikes listed, this tab also displays the
original row index of the parent sample.
• QC Duplicates and QC Dilutions display the % difference of the duplicate or dilution. For all QC
Duplicates and QC Dilutions listed, this tab also displays the original row index of the parent
sample.
• The Samples, Blanks, and Calibration Standards section displays the named information only where
a sample fails the QC criteria specified — Samples display sample concentration, IS % recovery,
RSD, and SD information; Blanks display measured intensity SD data; and Calibration Standards
display net intensity RSD data.
The categories are each displayed in their own collapsible tree format — click the + and -
signs beside each header to expand and view or collapse and hide the available data.
All QC types from the Method window QC tab are considered in this section. However, because the
QC Calibration sub-tab deals with limits on the calibration as a whole (such as slope, intercept, and
correlation coefficient limits) rather than on individual samples, no QC failure is flagged if an
individual calibration standard goes outside specified limits, and no data, sample names or analyte
headers appear in red if a calibration fails a QC check. When a calibration fails, the calibration
information is displayed on the Intensities, Concentrations, and Unfactored Concentrations tabs as a
Calibration Curve, and expanded upon on the QC tab with the addition of Slope, Intercept, and
Correlation Coefficient values for each analyte. Also note that repeated samples and diluted samples
as a result of QC failure actions are not added to this tab as QC Duplicates or QC Dilutions.
If a QC measure requires that there be a valid calibration in the current workspace, and none exists,
the QC Status column will appear blank, rather than showing Passed or Failed, and the relevant cells
on the QC tab will also appear blank, as no data could be properly calculated.
You can also access the data on this tab from any of the other tabular views where a QC Status cell
displays a Failed marker; simply click the Failed cell or the corresponding Sample ID to go to the
relevant row on the QC tab. Note that QC failure messages are not displayed on this view — to view
a failure message, you must look at the relevant individual Current Sample report.
You can display additional columns to show the acquisition date and time, and reprocessed
data flags for relevant samples — click Advanced to configure this option.
Data Viewer . 209
2. In the Sort Analyte header by drop-down list, select the type of sort order to use
for analytes in the Data Viewer table headers.
3. If you have enabled QC (Quality Control) checking in one or more of your methods,
and wish to display whether or not the QC measures have passed or failed on the
Intensities, Concentrations, and Unfactored Concentrations tabs, enable the Display
Quality Control Status check box . Whether displayed onscreen or not, QC
information is always exported with the sample data.
4. If you want to display the Sample Acquisition Date and Time on the Intensities,
Concentrations, and Unfactored Concentrations tabs, enable the Display Sample
Acquisition Date and Time check box. Whether displayed onscreen or not, time
and date information is always exported with the sample data.
5. To Indicate Samples Outside of Limits click this check box and select a color for
the Lower Limit and Upper Limit from the drop-down. The sample limits are
entered in the Sample Limits sub tab of the Method Editor Checks tab and are
shown based on the type of concentration selected.
6. To Display Autosampler Location click this check box. Adds a A/S Loc column
displaying the autosampler locations of all samples.
7. In the Intensity field, select the number of decimal places to display for Intensity
values. Valid values = 0-4
8. In the Concentration field: Select the number of decimal places to display for
Concentration values. Valid values = 0-4
210 . Syngistix™ Software Guide
9. In the RSDs field: Select the number of decimal places to display for RSD (Relative
Standard Deviation) values. Valid values = 0-4
10. In the % Recoveries field: Select the number of decimal places to display for
Percent Recovery values in general, and for Percent Difference values on the QC tab.
Valid values = 0-4
11. Click OK to save your changes.
Data Viewer . 211
Note: You do not need to have Microsoft Excel installed on the same computer as your instrument
software in order to perform a data export. If Excel is not installed, the export file will still be
saved with all applicable data, and with the Internal Standards graph drawn in .jpg form. You
can then transfer the file to another computer, or open the file with an Excel-compatible
reader.
At any point in your determinations, click the Export All... button to export all currently
available data from the Intensities, Concentrations, Unfactored Concentrations, Internal
Standards, and QC Data Viewer tabs to a Microsoft Excel compatible file. Each tab is given a
separate worksheet in the resulting .xls or .xlsx file.
Additional information, including the relevant dataset name, method name, QC pass/fail, and
time and date of acquisition, is also made available in the exported file to provide more clear
and complete sample identification, even though it may not be present in the onscreen
report views in the instrument software.
The default file format for the export function is .xlsx, but .xls is also generally available.
However, due to limitations in Microsoft Excel, if you are exporting more than 256 columns of
data, you can only export in .xlsx format.
Note: If you have a version of Microsoft Excel earlier than 2007 installed on your computer, you will
be allowed to save to .xlsx format, but you will not be able to correctly open the resulting file
in that version of Excel (the file will appear to contain garbage information). In this case, you
can choose to instead save to .xls format, which will open in any version of Excel, or you can
open the resulting .xlsx file in an Excel-compatible viewer or on another computer running
Excel 2007.
Tip: If you will be printing your exported reports to a black and white printer, append the mode
you are using to each analyte name in your method so that this information is included in
your print-outs (otherwise, mode is indicated by color only).
212 . Syngistix™ Software Guide
1. Next to Results Data Set Name, click on the file icon and select a results data set
that contains the data you want to reprint.
2. Next to Analysis Batch Date/Time, click on the file icon and select a batch that
you want to reprint. The Select Analysis Batch dialog appears and displays the
batches that are available in the data set you selected. Batches are identified by the
date and time they were initially created.
The rules for how batches are created are as follows:
• When you are performing Manual Analyses, a batch is created when you run the
first solution after opening the Manual Analysis window. The batch will end when you
close the Manual Analysis window. All samples that are run in between are stored as
part of the same batch.
• When you are performing Automated Analyses, a new batch is created when you
first select one of the analyze buttons (Analyze All, Calibrate, and Analyze Samples).
The batch will end when you close the Automated Analysis Control window. If the
analysis is paused and then continued, the continuation of the analysis will be part
of the same batch.
• When you are Reprocessing Analyses a new batch is created when you first
open the Data Reprocessing window and click the Reprocess button. The batch
will end when you close the Data Reprocessing window.
3. Click Preview to preview the selected data in the Results window, without printing.
4. Click Print to print the selected data.
Output is sent to the Results window. It should be noted that no new data is stored
to the Results database when you use the Reprint function.
Devices
214 . Syngistix™ Software Guide
P um p Control
You use this dialog to select options for the peristaltic pump.
To display this dialog:
1. On the Instrument tab, click on Devices.
The devices screen appears.
2. Click the Pump tab.
Pum p Settings
Tubing: Select the tubing type from the drop-down list, for example:
• black/black
• orange/red
• orange/blue, etc.
The pump tubing selected will determine the pump speed needed to achieve a given sample
flow rate.
Flush Rate: Enter the default flush speed. This is the pump speed that will be used when you
click on the Flush button in the Plasma Control window. A sample flush is normally used to
deliver sample from the sample vessel to the nebulizer at a faster rate than the normal sample
flow rate. This decreases the total amount of time it takes to analyze each sample.
Enable Tubing Saver: Select this check-box to use the Tubing Saver feature, which extends
the lifespan of the peristalic pump tubing by operating the pump at a slower speed than normal.
Devices . 215
M odel
The autosampler model was set up when the software was installed.
To change the model, exit the software and run the Reconfigure utility.
To run the Reconfigure utility, click on Start All Programs PerkinElmer
Syngistix for ICP Reconfigure.
Tray Type
Select the tray type that corresponds to your autosampler configuration.
To flush at start of analysis (displayed only when an ESI with prepFAST is installed and
configured):
Select this checkbox to have the ESI with prepFAST system flush at the start of an
analysis.
Rinse Options
The Rinse options display for those autosamplers that have a rinse ___location used to rinse
the sample probe. If you want to change the rinse solution continuously, select one of the
options where the pump is switched on. Use a higher Pump speed to change the rinse
solution more quickly.
Select from the following rinse options:
Pump always off: The rinse pump is always switched off, even when the sampling probe is
in the rinse ___location. When this option is active, other rinse pump options cannot be selected.
Pump always on: The rinse pump runs continuously.
Pump on while probe in rinse loc: The rinse pump is on for the dwell time that the
sampling probe is in the rinse ___location. The dwell time is preset in the operating software and
cannot be changed by the user.
Pump on while probe in rinse loc. plus xx seconds: The rinse pump is on for the dwell
time that the sampling probe is in the rinse ___location; it continues to pump for the number of
seconds entered in the entry box after the sampling probe has been raised out of the rinse
___location.
Pump on when probe in rinse loc. for xx seconds: The rinse pump starts when the
sampling probe enters the rinse ___location and pumps for the number of seconds entered in
the entry box. This time can be longer or shorter than the default dwell time of the probe in
the rinse ___location.
Devices . 217
FIAS
You use the FIAS Control window to manually control the FIAS pump module and view the
progress of the FIAS program. The status of the FIAS pump module and the FIAS program
are shown at the top of this window. The FIAS On/Off and Goto Next Step buttons will
always be disabled since there is no FIAS program in this configuration. You can only use
these controls when there is no analysis in progress.
To replum b the tubing for operation of the peripum p w ithout HTS (that is,
the HTS disabled):
1. Disconnect the autosampler probe from valve position #1 and attach it where the
carrier line connects to the black/black sample tubing before the peripump. You will
need to disconnect the carrier line at the peripump and set it aside.
2. Disconnect the nebulizer line from valve position #5 and attach it to where the
carrier line connects to the black/black sample tubing after the peripump. You will
need to disconnect the carrier line at the peripump and set it aside.
Note: This carrier line is the short one that connects to valve position #4.
220 . Syngistix™ Software Guide
R em ote Trigger
The Remote Trigger capability is only available for the Avio series and Optima 5000 and
above running in the Continuous technique.
To display this item:
1. On the Instrument tab, in the Devices group, click on Devices.
The devices screen appears.
2. Click the Remote Trigger tab.
A Quick Look
To display this window
On the Instrument tab, click Plasma Control.
Hint: You can press F9 to turn the plasma on and off even if the Plasma Control window is not open.
The Plasma Status window indicates if ignition is successful or if there is a problem. For more
information, see System Monitors. For details about the ignition process, see Igniting the
Plasma. Wait one hour before analyzing samples. This warm-up time ensures accuracy in
Hardware Control Windows . 223
your results since it allows the temperature of the sample introduction system to fully
stabilize.
Override Method
If this box is checked, the instrument will use values for your next analysis as specified in this
window. If the box is not checked, the instrument will use the values in the active method.
Selecting Override Method does not change the values in the active method or the method
stored in the results library.
Gas Flows
If you select the Override Method checkbox, the Plas, Aux, and Neb buttons allow you to
change the post-ignition flow rates of the argon gases and to monitor their current values.
Plas, Aux, and Neb refer to the plasma, auxiliary, and nebulizer gases. The blue numbers in
the display indicate the current flow rate.
• To start or stop gas flow, click on the desired button beneath the display. The green
light on a gas button indicates that the gas is flowing.
• To change a gas flow rate, select or type a value in the box beneath the appropriate
gas display. For more information, see Recommended Settings for Plasma
Parameters and Recommended Settings for Nebulizers. The maximum flow rate that
you can enter cannot actually be attained by some nebulizers. If the nebulizer cannot
reach the highest value, it will return the value it reached to the display. An error
message will be recorded on the Plasma tab of the Instrument Diagnostics window.
• Click on Apply after you have adjusted the setting for the flow rates.
RF Power
These allow you to change the radio frequency power that is dissipated in the plasma and to
monitor the current power.
• To change the power setting, select or type a value. For more information see
Recommended Settings for Plasma Parameters. Click on Apply after you have
adjusted the RF power.
Pump and Flush
These allow you to change the sample flow rate and to monitor the status.
• To change the sample flow rate, select or type the appropriate value. The software
adjusts the pump speed based on the type of pump tubing you selected in the Pump
Configuration dialog. To change the pump tubing, in the Options menu, click on
Pump. A typical sample flow rate is 1.5 mL/min for all instruments. Ranges for
sample flow rates vary with the pump and pump tubing you are using. For example,
values are from 0.6 to 5.7 mL/min for the PerkinElmer pump (with 0.76 mm i.d.
tubing) and from 0 to 2.5 mL/min for the Gilson pump. Then, click on Apply. For
more information, see the Configure Pump dialog.
• Click on Pump to start or stop the peristaltic pump. The green light indicates that
the pump is turned on.
• Click on Flush to set the pump speed to the flush setting in the Pump Configuration
dialog.
224 . Syngistix™ Software Guide
Auxiliary Flow: 0.2 L/min 0.2 mL/min 0.5 mL/min 0.5 mL/min
Nebulizer Flow: 0.80 L/min 0.70 L/min 0.50 L/min 0.50 L/min
(for Low-Flow GemCone or the
Concentric Glass nebulizer)
Sample Flow Rate: 1.50 mL/min 1.0 mL/min 0.80 mL/min 1.0 mL/min
Hardware Control Windows . 225
A Quick Look
To display this window
On the Instrument tab, in the Spectrometer group, click on Spectrometer Control.
Simultaneous ICP Spectrometers
The Spectrometer Control window is shown below as it appears for simultaneous ICP
spectrometers and is set for radial viewing.
Note: In the Transient technique the following buttons: Align View , W avelength Calibration, and
Hg R ealign buttons are not displayed since they are not applicable to FIAS.
226 . Syngistix™ Software Guide
For radial viewing, you can modify: For axial viewing, you can modify the
• the viewing position from the RF coil to viewing position relative to the plasma
the tip of the plasma . (horizontal scale center on two axes.
0 to 30 mm)
• the position relative to the plasma
center (vertical scale -10 to 10 mm)
Hardware Control Windows . 227
To use the new settings in place of the settings in the method, select Override Method.
The settings for both coordinates will be used. If you do not select Override Method, the
system will use the setting for the Viewing Distance parameter. This parameter is in the
method on the Sampler: Plasma page. It has only one coordinate and assumes the other
coordinate to be 0. For example, a setting of 15.0 indicates the coordinates of 15.0 and 0.0.
If you want to set the torch viewing position individually for each analyte, you can do this
using the Viewing Distance parameter in the method.
Click on the Select Analyte option and then select another element from the
drop-down list. This feature is for specialized analyses where you want to
optimize the intensity for an individual analyte of interest. This may adversely
affect the intensities of other analytes.
-or-
Click on the Other option and type in an element and/or wavelength not in the
drop-down lists.
Note: If you have an ESI with prepFAST installed and configured, specify the Autosampler Location
of the solution.
Note: If you have performed the procedure above, but are not satisfied with the results, you can
perform an Extended Search over a larger area.
9. Click Extended Search (For axial viewing only) and repeat the procedure above to
perform a search over a larger area of the torch.
Note: This search takes longer than the usual procedure. Before using Extended Search, you
should perform the sodium bullet test to make sure that the sample is reaching the plasma.
If any of the following conditions are found, a message dialog appears to give you an
opportunity to confirm that you wish to use the new alignment (or cancel it) if desired:
• The distance from the last alignment is greater than 5 mm.
• The value of the peak is less than 10,000 counts.
• The element wavelength used for the last optimization is not the same as the one
used for the previous optimization.
improve sensitivity for elements with wavelengths below 190 nm since oxygen absorbs below
190 nm. On scanning CCD ICP spectrometers, you have the option of turning the purge gas off.
View Mode (Dual View instruments only)
Select the plasma viewing mode.
Radial: Light emitted from the side of the plasma passes through the torch slit and is
directed to the spectrometer optics.
Axial: Light emitted along the axis of the plasma is directed to the spectrometer
optics. The observation zone of the plasma is circular and the spectrometer views a
column of light from the central channel of the plasma.
Attenuated (Attn) Radial or Attenuated (Attn) Axial
These settings are available only for scanning CCD ICP spectrometers. Use these settings
when lower intensities are desired, for example, for samples of high concentration that would
normally saturate the detector and for sensitive wavelengths, typically in axial mode.
Shutter Auto/Closed/Open
A shutter in the transfer optics allows light from the plasma to enter the spectrometer optics.
This shutter may be set to the Auto, Closed, or Open position. The Auto setting indicates that
the shutter is under instrument control.
Usually, the shutter is set to Auto. If you have an extensive number of samples to analyze,
however, you may wish to set the shutter to the open position manually to increase
analytical throughput. Be sure to close the shutter when the analysis is complete.
Leaving the shutter in the open position with the plasma on could lead to
deterioration of the optics and eventual degradation of UV performance. It is
recommended that the shutter be closed when analyses are not being performed.
To measure dark current, take measurements with the shutter in the closed position.
Hg Lamp Off/On
This control appears only for simultaneous ICP spectrometers. An internal mercury lamp,
under system control, is used for the mercury realignment procedure and periodic mercury
recalibration. Manual control of this lamp is available for diagnostic purposes to verify that
the signal is reaching the detector and that the mercury lamp is working.
Torch Viewing Position: To The View Dist (Viewing Distance) parameter is set in
change the position, select new the method on the Sampler: Plasma page.
coordinates and click on Apply. The Viewing Distance parameter has only one coordinate
For either axial or radial viewing, and assumes the other coordinate to be 0. For example, a
both coordinates will be used. setting of 15 indicates the coordinates of 15 and 0.
To override a setting in the method, select the Override Method box next to the setting in
the Spectrometer Control window.
230 . Syngistix™ Software Guide
Wavelength Gathers data for UV or VIS emission lines to The instrument must be operated with the
Calibration compensate for slight variations in optical plasma on for at least one hour before
alignment. At the end of the UV or VIS initiating wavelength calibration on a
(sim ultaneous wavelength calibration, the system spectrometer.
spectrom eters) determines the wavelength offset of an
emission line from the internal mercury lamp Perform this procedure:
and records the slit position as a reference • when the instrument or software is first
point for future mercury realignments. installed
• when the instrument is moved to a new
___location
• after reinstalling or upgrading the
software
• if analyte peaks in the Examine Spectra
window are significantly offset from the
central line for the wavelength on a
consistent basis
Initialize Optics Performs a prism scan to optimize The instrument must be operated with the
wavelength for the slit in the instrument plasma on for at least 10 minutes before
(scann ing CCD optics. The system takes an intensity reading, initializing optics.
spectrom eters) scans the surrounding intensity range and
locates the midpoint. If this midpoint varies Initialize Optics is performed automatically
from the initial intensity measurement, the during analyses. However, if there are wide
system will optimize optics for use in fluctuations in ambient laboratory
subsequent analyses. temperature that appear to affect intensity,
you can initialize optics manually. To do
this, click on the Initialize Optics button in
the Spectrometer Control window.
Hg Realign To compensate for spectrometer drift (for The spectrometer must be in the ready
example, changes in barometric pressure), mode before initiating a mercury
(sim ultaneous the system compares the mercury slit realignment.
spectrom eters position recorded at the end of the
only) wavelength calibration to the current position Use before adjusting the peak wavelength,
found on the detector. a procedure which allows you to fine-tune
the calibration for a particular wavelength.
For more information, see Adjusting the
Wavelength.
Use before collecting data for MSF models.
Notes: If your peaks are slightly offset, a system wavelength calibration is usually not necessary.
Instead, fine adjustments to wavelengths can be made using the Examine Spectra window.
For more information, see Examine Spectra Window.
If using MSF and a wavelength calibration is performed, you must update the instrument and
data set. The MSF models must then be recreated before performing an analysis for accurate
results. Failure to do so will result in MSF not being calculated for certain wavelengths.
Im portant: Since spectrometers are sensitive to thermal effects, it is important that the instrument
be operated with the plasma on for at least 30 minutes before initiating wavelength
calibration on a spectrometer.
Note: If you have an ESI with prepFAST installed and configured specify the Autosampler Location
of the solution on the Wavelength Calibration dialog.
1. Aspirate the Calmix 3 solution (Part No. N0582152). In a HTS system, remove the
carrier line from the carrier bottle and place it in the UV wavelength calibration
solution.
Note: On Axial (XL) instruments, you may need to dilute the wavecal solution 1:10 to keep certain
emission lines from saturating the detector. On Dual View (DV) instruments, select Radial
viewing. If you have selected axial, a message appears informing you to change to radial.
If these specifications are not met, repeat the wavelength calibration and make sure all
peaks can be seen in the Spectra Display window. If the specifications are still not met, a
complete optical alignment may be required. Contact your PerkinElmer service engineer.
For spectrometers that have a visible wavelength channel on the detector, to
perform VIS channel wavelength calibration:
1. Aspirate the VIS Wavecal mix (Part No. N9302946). In a HTS system, remove
the carrier line from the carrier bottle and place it inthe UV wavelength calibration
solution.
Note: On Axial (XL) instruments, you may need to dilute the wavecal solution 1:10 to keep certain
emission lines from saturating the detector. On Dual View (DV) instruments, select Radial
viewing. If you have selected axial, a message appears informing you to change to radial.
complete, the VIS coefficients and RMS (Root Means Square) value will be displayed
in the Results window. These values should meet the following specifications.
If these specifications are not met, repeat the wavelength calibration and make sure all
peaks can be seen in the Spectra Display window. If the specifications are still not met, a
complete optical alignment may be required. Contact your PerkinElmer service engineer.
Note: In the Automated Analysis Control window, you can specify a mercury realignment (called
Auto Wavelength Realign) to occur at defined intervals during an automated analysis (one-
hour intervals are recommended). For more information, see Autom ated Analysis
Control: Set Up P age.
Note: On scanning CCD ICP spectrometers, a detector calibration is performed automatically when
you start the software and takes 15 to 30 seconds.
6. Open a method that contains at least one analyte with a valid calibration curve. The
equation used cannot be Bracketing or Method of Additions.
7. Click OK on the Performance Checks dialog to begin the Detection Limit analysis.
The Performance Checks dialog closes and the Detection Limit Checks analysis
begins.
FI AS Control W indow
You can use the FIAS Control window to control the valve, pumps, and remotes independent
of any other ICP functions.
• ICP peristaltic pump. If you do not want to use the ICP peristaltic pump while
using the FIAS, you must turn it off manually by setting the pump speed to 0. In this
case, 0 should be considered a valid speed; no functionality should be disabled due
to a speed of 0.
• Startup/Shutdown. The Pumps Off At End feature (which automatically turns
the FIAS pumps off at the end of an analysis), is not used in ICP. Of course, as
described above, if the plasma is automatically shut down at the end of an analysis,
the FIAS pumps will be turned off as part of that process.
I nform ation Display W indow s
238 . Syngistix™ Software Guide
Note: If you attempt to open the Continuous Graphics window when no analytes are defined in the
current method, the Open Method dialog displays. This prompts you to open a method with
at least one analyte defined before going into Continuous Graphics.
Analyte Table
Analyte: Displays the analyte names (as defined in the method).
Signal: Shows the current signal value for each analyte.
Visible: Shows whether each analyte is visible on the graph (checked), or is hidden (unchecked).
Style: Shows the line type and color for each analyte displayed on the graph.
Factor: For each analyte, the factor multiplied by the signal before it is displayed and graphed.
Offset: For each analyte, the offset added to the signal before it is displayed and graphed.
Select Analytes Button: Opens the Enable/Disable Elements dialog.
Note: It must be less than the M ax limit minus the minimum height of the graph (a value of 10)
240 . Syngistix™ Software Guide
• Display Options: Click this button to open the Continuous Graphics Options dialog.
• Print: Click this button to print an image of the window; similar to the printing
format of the Examine window.
• Auto Expand Graph: Sets the maximum value on the y-axis to about 10%
greater than the highest current signal value of any analyte.
• Auto Zero Graph: Sets the current signal of each analyte to zero.
• Set Graph Maximum: Sets the graph to its maximum size.
2. Click Display Options to display the Continuous Graphics Options dialog.
Note: If you choose a line type other than solid, the line width must be set to 1 for
the line to be rendered in the desired style.
Set Defaults: Click to restore the line options to their factory preset values.
• Colors Tab - Set the colors for the components of the graph on this page.
Define the colors for the components of the graph on this page.
Background: Click on the color tab under Screen to select the background
color of the graph.
Axes and Labels: Click on the color tabs under Screen or Printer to select
the colors for the axes and labels.
Screen: Select the colors for an on-screen plot.
Printer: Select the colors that will be printed on a color printer.
Defaults: Click this button to restore the screen color options to their
factory preset values.
242 . Syngistix™ Software Guide
3. In the Print dialog that appears, check that the correct printer is shown. If you need
to select another printer, click the drop-down arrow next to the Printer Name field.
Click on the Printer name to select it. To change other setup options such as the
paper size, click on Properties.
4. Click on OK to start printing.
The Spectra Display window always uses a layout of three rows and two columns for
printouts. Changing the layout on the screen will not affect the printout. Up to six
spectra are printed on one page.
When you print the Examine Spectra window, the spectra are overlaid in one graph
on the page.
Information Display Windows . 243
Results Options
To display the Results Options dialog:
Right-click in the Results window and select Display Options.
The Results Options dialog appears.
2. After you have made your selections, click on OK to close the dialog.
Select Show Unpopulated Fields for Sample Wt., Initial Sample Vol., Dilution,
Sample Prep. Vol, Autosampler Location, and Analyst from the sample header in the
results log for all sample types.
Note: Blank spaces replace the field label for an unpopulated field value on lines that have multiple
fields. Also, those lines where all fields are unpopulated will not be displayed.
Printing
To print this window:
All information shown in this window can be printed as follows:
• automatically (See Printing Results for further information), or
• From the Syngistix Application button select Print Active Window (while the
Results Display window is opened). Then select Quick Print or Print Preview.
Tip: When you clear the Results Display (on the Results tab in the Results group click Clear), the
contents are written to a log file called results.log in the user's home directory (for example,
C:\Users\Public\PerkinElmer\Syngistix\ICP\SystemFiles\Temporary Files). This log file is
erased each time you restart Syngistix. A log file is an ASCII text file that can be printed,
modified in a text editor (e.g., Notepad) or saved.
Note: The Results Display window can only contain 2000 lines of information at a time
(approximately 12 pages). When the 2000-line limit is exceeded, new lines are added at the
end of the display and old lines are removed from the beginning. The lines removed from the
display are stored in results.log under the user's home directory, for example: C:\pe\Default
User\Temporary Files\Results.log.
Tip: To obtain the most abbreviated list of results, select only Means and Statistics from the
M ethod Editor Options page.
Information Display Windows . 245
Select the type of information you want to include in the Results Display and the Printed Log
for your analysis.
Analytical Header: Select this to include a header when a new analysis is begun. A
new analysis header is also displayed each time the current method is modified and
another sample is analyzed.
Method Header: Select this to include a header that contains information on the
method. Select short or expanded.
Sample Header: Select this to include a header with sample information. Click the
checkbox if you want to start each sample on a new page.
Replicate Data: Select this to include data for each replicate.
Means and Statistics: Select this to include the mean values of each set of replicates
and to include the standard deviation, relative standard deviation, and the residual error.
You must have means selected in order to display statistics.
Auto Integration Report: Select this to include auto integration data for each
measurement when auto integration is being used.
Display over calibration message: Select this option to display an over calibration
message when the sample concentration is greater than the entered percentage of the
highest standard. When this option is checked the % spin box is enabled. In the % spin
box enter a value between 100 and 999 %.
Analysis List: Select this option to include a summary of the operations that were
performed on all of the samples.
Matrix Test Reports: If there is a sample matrix, mark this box to include matrix
reports.
Calibration Summary (Auto Analysis only): Select this to include a calibration
summary in the Results Display window. If this is selected, the calibration summary is
automatically included for automated analyses after the last standard is analyzed. Note:
For manual analyses, you must select the Calibration Summary command in the Analyses
menu.
Detailed Cal. Summary: Select this option to display a detailed summary of each
calibration curve, including the calculated concentration of each standard. This summary
will be displayed after the final standard has been run.
Save with Results - Spectral Data: Select this to include the spectral data in the
results data set. The spectral data must be stored in a results data set if it is to be
displayed in the Examine Spectra window or used for setting up MSF models or Data
Reprocessing.
Remarks: Use this entry field to type your comments regarding the method.
Note: The Results Display window is not cleared automatically when you start a new analysis. To
clear the window, on the Results tab in the Results group click Clear.
246 . Syngistix™ Software Guide
Analytical Header
A discussion of each entry from the Analytical Header appears below:
Start Time: The date and time when the current analysis began.
Note: To set the format for Date/Time, click on the Windows Start menu button point to
Settings, and then click Control P anel. In the Control Panel window, click the Date/ Time
icon and enter the information in the dialog box.
Logged In Analyst: The name of the Analyst taken from the Windows system log in.
Spectrometer Mode: The Spectrometer Model selected in the current configuration.
Plasma On Time: The time the plasma was ignited.
Technique: The name of the sampling technique selected in the Select Sampling
Technique dialog. (ICP, Continuous, Transient.)
Autosampler Model: The type of Autosampler model you are using.
Sample Information File: The name of the Sample Information File (.sifx file) and the
full pathname.
Results Data Set: The name of the Results Data Set. A Data Set contains the essential
components of an analysis, i.e. the Method, the spectral data, Sample Information and
the analytical results. You specify the Results Data Set name when any one of the
following actions is performed:
• Manual Analysis Control window → Results Data Set Name (Open button) →
Results Data Set dialog
• Automated Analysis Control window Set Up tab →
Results Data Set Name: (Open... button) → Results Data Set dialog
• Data Reprocessing window → Save Results in Data Set (Open... button) →
Results Data Set dialog
Note: Look at all of the selections on the Options page in the Method Editor window to get an
overview of the selected Analytical Results that will appear in the Results data set or the
Results window.
Results Library: The name and ___location of the Library where the Results are saved.
Information Display Windows . 247
Note: To set the format for Date/Time, open the Control Panel window and double-click on the
Date/Time icon.
Sample Concentration Units: For each sample, the mean sample concentration
expressed in sample units.
%RSD: For each sample, the %RSD of either the corrected signal and the mean
standard (or sample) concentration.
Residual Error: The amount the calibration standard deviates from the entered
concentration as a percent.
Information Line: Additional information about the sample measurements that may be
of interest to you, e.g., standard applied, QC messages (including QC recoveries), etc.
Note: To set the format for Date/Time, click the Start button, point to Settings, and then click
Control P anel. In the Control Panel window click the Date/ Tim e icon and enter the
information in the dialog box.
Sample Prep Volume: After a solid sample has been dissolved or a liquid sample has been
acidified (or otherwise treated) the resulting solution is prepared to a specific volume. This is
the Sample Prep Volume. The information is from the Sample Information File.
Data Type: Original or Reprocessed.
M ethod Header
You can display a short or expanded method header in the Results Display window. Make a
selection in the Method Editor Options tab.
A discussion of each entry from the Method Header appears below.
Method Name: The method name used for the analysis. You specify this name in the
Save Method As dialog when you select Save As... from the Save drop-down in the
Method group.
IEC: The name of the Interelement Correction File (.IEC file) will appear only if you
make the appropriate selections: Method Editor → Process page → Spectral
Corrections tab (select IEC for an element under the Overlap Correction Column and
select an IEC Table) and Results are saved.
Method Description: A brief description of the method used for the analysis. You
specify this name when you select: Method Editor window → Spectrometer page
→Define Elements tab → Method Description
Information Display Windows . 249
Method Last Saved: The date and time of the method was last saved.
MSF: The name of the Multicomponent Spectral Fitting File (.MSF file) will appear only if
you make the appropriate selections: Method Editor → Process page →
Peak Algorithm..., tab (select MSF for an element under the Peak Algorithm Column).
Also select an MSF Table on the Spectral Corrections page.
Method Header Expanded: The Expanded Method Header contains all the above
entries, plus the additional entries listed below.
Analyte: The name of the element analyzed. The element symbol is shown along with
the emission wavelength that was used. The element and wavelength are taken from the
active method.
Calib Eq'n: This is the calibration equation that is specified in the current method. (A list
of calibration types is shown on the Calibration page of the Method Editor window.) After
the calibration curve has been determined, you can clear (delete) the calibration by
clicking on Clear Calibration Blank from the Analysis menu.
Processing: Peak area, peak height or MSF.
View: Plasma viewing condition: Attenuated Axial or Attenuated Radial.
Internal Standard: Lists the name of the Internal Standard as it appears on the
Spectrometer pages, Define Elements tab. If there is no Internal Standard, then None or
N/A is displayed.
IEC: InterElement Correction, Yes/No.
Note: The value will always be 1.000000 if your calibration curve has only two points (calibration
blank and 1 calibration standard).
250 . Syngistix™ Software Guide
Reslope: The reslope standard is used to make small corrections to the slope of the
calibration curve. Usually, a calibration blank is analyzed just before the reslope
standard. The new reslope value is then compared with a multipoint curve. Reslope is a
time-saving device that lets you adjust a curve without running multiple calibration sites.
The application uses the new curve (reslope) to determine the concentration values.
Note: The value will always be 1.000000 if your calibration curve has only two points (calibration
blank and 1 calibration standard).
Slope: The calculated slope of the calibration curve. Slope represents the relationship of
the increase in intensity to the increase in concentration. It is the ratio of the change in
the y-axis to the change in the x-axis
Intercept: The calculated y-intercept of the calibration curve. The y-intercept is the
point where the calibration curve crosses the y-axis of the calibration plot. It represents
zero concentration.
Printing R esults
You can automatically send a hard copy report of the analytical results to the printer as the
results are generated.
Note: If you want to be certain that all of the analytical results generated by the spectrometer are
documented you are encouraged to print a log during the analysis.
click on the check-box if to select it. You must have a printer online. The default
printer is automatically selected. Options for the printed log can also be selected on
the Options tab of the Method Editor.
252 . Syngistix™ Software Guide
Note: On scanning CCD ICP spectrometers, you have the option of using Attenuated Axial or
Attenuated Radial as the plasma viewing type in the method. Use these settings to provide
lower intensities for samples of high concentration that would normally saturate the detector
and for sensitive wavelengths.
Saturation Codes
The software provides the following saturation error codes or messages. In some cases,
saturation is indicated during "preshot." This is an initial reading that is taken to determine
the optimum auto-integration time. On the Options page of the method you can select Auto
Integration Report which will give you the exact integration times determined during "auto-
integration" or "pre-shot."
Information Display Windows . 253
Code Description
2 "Saturated2" appears in the Net Intensity column in the Results Display. This
information also appears in the Spectra Display window. This code and message applies
only to simultaneous ICP spectrometers.
The intensity measured during pre-shot is too high for several wavelengths and the
detector cannot read out the data. You may be able to rerun the analysis and select
only one of the wavelengths to prevent saturation from occurring.
3 "Saturated3" appears in the Net Intensity column in the Results Display. This
information also appears in the Spectra Display window.
The intensity measured for the analyte during pre-shot is too high, even for a 1 ms
integration (the shortest integration time available). Either the wavelength chosen for
the analyte was too sensitive or the sample contained too high a concentration of the
analyte.
4 "Saturated4" appears in the Net Intensity column in the Results Display. This
information also appears in the Spectra Display window.
The intensity measured for the analyte during the replicate readings is too high. This
may have occurred because the signal wasn't stabilized before the pre-shot
measurement, so the signal intensity changed between the "pre-shot" reading and the
time the replicate was measured.
For the Optima 7300/8300 and Avio 500, Avio 550 Max, Avio 560 Max, in manual
integration, the message "Saturation within survey window" appears in the Results
Display. For either type of integration, the message "Saturated. Code = 4" appears in
the Spectra Display.
First, try increasing the read delay and rerunning the analysis. If saturation still occurs,
the wavelength chosen for the analyte was too sensitive or the sample contained too
high a concentration of the analyte.
5 In automatic integration, the message "Saturation outside of integration window"
appears in the Results Display. A peak with too high an intensity was found outside of
the auto integration window but within the survey window.
For the Optima 7300/8300 and Avio 500, Avio 550 Max, Avio 560 Max in manual
integration, the message "Saturation within survey window" appears in the Results
Display. For either type of integration, the message "Saturated. Code = 5" appears in
the Spectra Display.
For more information on the integration and survey windows, refer to the Spectral
Windows page in the Method Editor.
The saturated peak may not be the analyte of interest, but an interferent. If you are
using background correction, be sure to check that the background correction points
are not placed in the range where saturation is occurring, which can invalidate your
results.
6 In automatic integration, the message "Saturation outside of integration window"
appears in the Results Display. In manual integration, the message "Saturation outside
survey window" appears in the Results Display. A peak with too high an intensity was
found outside the Survey window. For either type of integration, the message
"Saturated. Code = 6" appears in the Spectra Display.
For more information on the integration and survey windows, refer to the Spectral
Windows page in the Method Editor.
The saturated peak may not be the analyte of interest, but an interferent. If you are
using background correction, be sure to check that the background correction points
are not placed in the range where saturation is occurring, which can invalidate your
results.
254 . Syngistix™ Software Guide
Reslope
Run a calibration curve with two or three standards (a multipoint curve). Use Reslope to
determine a new value for the curve to compare it with the multipoint curve. The reslope
curve, which appears as a dashed line, lets you adjust a curve without running multiple
calibration sites. The application uses the new curve (reslope) to determine the concentration
values.
Information Display Windows . 255
Calib Eq'n
This is the calibration equation that is specified in the current method. (A list of calibration types is
shown on the Calibration page of the Method Editor window.) After the calibration curve has been
determined, you can clear (delete) the calibration by clicking on New Calibration in the
Calibration group.
Corr. Coeff.
The correlation coefficient indicates how well the data fit the generated calibration curve. A
value of 1.0000 would indicate a perfect fit.
3. In the Print dialog that appears, check that the correct printer is shown. If you need
to select a different printer, click the drop-down arrow next to the Printer Name field.
Click on the Printer name to select it. To change other setup options, such as the
paper size, click on Properties.
4. Click on OK to start printing.
The calibration curves are always printed in a layout of two columns and three rows. Changing
the layout on the screen will not affect the printout. Up to six calibration curves are printed on
one page.
256 . Syngistix™ Software Guide
Note: In the list of autosampler locations and solutions, the method is not shown for samples (unknowns).
3. Clicking on the Location column header shall sort the list by ___location.
4. Clicking on the Method column header (while in multi-method mode) sorts the list by
method.
Note: If a change is made to the method, SIF, or Auto Analysis window which affects the contents
of the Loading List, the Loading List window is automatically updated.
5. To print the list, right-click and then click on Print Autosampler Loading List or
click on the button and select Print Active Window. In the print dialog that
appears, select your printer and click on OK.
Ex am ine
Spectra/ M SF/ Transient Peak s
W indow
258 . Syngistix™ Software Guide
Overview of Ex am ine
The examine window displayed is dependent on the technique you are using.
• If you are using the Continuous Technique, you will see the Examine/MSF window.
• If you are using the Transient Technique, you will see the Examine Transient Peaks
window.
Overview of Ex am ine/ M SF
This window serves a dual purpose:
• You can examine the spectra that have been saved to a data set.
• You can correct for spectral interference by setting background correction points or by
using the MSF (Multicomponent Spectral Fitting) technique.
Refer to About Interference Correction for more information on the different ways you can use the
software to correct interferences.
To display this window
On the Results tab, in the Examine group, click on Examine.
Note: If this file has been modified but not saved, the file name in the dialog header will have an
asterisk ( * ) displayed to the right of the name. Once the file is saved, the asterisk will be
removed.
For more information on using this window in Examine Spectra mode, see Examine Spectra
Window.
To change this window to Examine MSF mode, select MSF from the drop-down list in the
top-left corner of the window. For more information on using MSF, see Overview of How
MSF Functions.
Examine Spectra/MSF/Transient Peaks Window . 259
Using the Ex am ine Transient P eak s w indow for the first tim e
By default, this window opens in the Examine Transient Peaks mode. In this mode, the word
Examine Transient Peaks is displayed in the top-left corner of the window. In Examine
Transient Peaks mode, you can:
• modify method parameters directly from the Examine window.
• modify the appearance of the spectra to aid in method development.
• set up spectral displays for reports.
Note: If this file has been modified but not saved, the file name in the dialog header will have an
asterisk ( * ) displayed to the right of the name. Once the file is saved, the asterisk will be
removed.
260 . Syngistix™ Software Guide
The main function of the Examine Spectra window is to display spectra that were saved to a Data
Set so that you can:
1. Modify Method parameters:
• Select Peak Wavelength and Background Correction Points directly from the graphic
display.
• Select Peak Algorithm (peak height or peak area) and the Points/Peak based on your
observation of spectra in the Examine Spectra window.
• Refer to the Update Method Parameters dialog.
2. Change the presentation of the spectra to aid in Method Development so that you can
identify interferences and select appropriate wavelength(s) for an element, etc.
3. Set up spectral displays for your printouts.
4. Troubleshoot possible hardware problems by evaluating standard spectra. (e.g., not
enough sample entering plasma, clogs, etc.)
5. Fine-tune the instrument wavelength calibration.
6. Correct saturated data. See Correcting Saturated Samples for more information.
To display this window:
On the Results tab, in the Examine group, click on Examine.
Note: If this file has been modified but not saved, the file name in the dialog header will have an
asterisk ( * ) displayed to the right of the name. Once the file is saved, the asterisk will be
removed.
Tip 2: Save the m ethod, if you wish to retain the changes made to method parameters from the
Examine Spectra/MSF window.
Tip 3: Save spectra to the same data set if you will want to overlay these spectra in the same display
because you can select only one Data Set per Examine session.
Examine Spectra/MSF/Transient Peaks Window . 261
M enus
Examine or MSF: Select either Examine or MSF to toggle the window between two different
modes.
Data menu Line menu Method menu Graph menu Replicates List
(This menu is Average, First, or
present only in Last
Examine mode.)
List of analytes button. Click this button to view a list of selected analytes. You can select any
analyte from the list to display it.
Layout
To select a display layout:
To use the default layout of all spectra, place a check mark next to Auto-Layout. An
appropriate number of rows and columns will automatically be selected to display all the
spectra. For example, if there are 11 analytes, Auto Layout displays a 4 x 3 grid.
To customize row and column layout, first remove the check mark next to Auto-Layout.
Then click on the counter spin buttons to specify the number of Rows and Columns in
the display. The number of rows and columns each range from 1 to 16, which means that
1 to 256 panes can be displayed at once.
262 . Syngistix™ Software Guide
Selecting Colors
Note: To return to the original screen colors, click on the Screen button under Default Color Settings.
-or-
If you are satisfied with the colors, click on OK to apply the changes and close the dialog.
Printing Spectra
To create a printout of the spectra, click the Application button, select Print Active
Window, and select Quick Print or Print Preview. The spectra are printed in black and
white or in color, depending on the type of printer you have. See Printing Spectra.
Displaying MSF Analyte Spectra
To display the corrected MSF analyte spectra, select the Enable MSF analyte spectra
checkbox on the bottom of the Colors section. You can then view the corrected MSF
spectra in comparison with the uncorrected spectra.
Return to the Default Colors
To change all of the screen colors or printer colors back to their default settings, select the
Defaults buttons under the Screen or Printer columns.
To change the colors without closing the Spectra Display Options dialog, click on Apply.
-or-
To apply the change and close the dialog, click on OK.
Spectra
MSF spectra line width – All other spectra line width
To select line widths for displaying spectra, type a number from 1 to 10 to designate the
relative line width for MSF Spectra and for All Other Spectra.
MSF Spectra Line Width defaults to 1 and All Other spectra Line Width defaults to 2.
Return to the Default User-Configurable Options
To change all of the user-configurable options (other than the colors) in this dialog back to
their default settings, click the Defaults button.
To change the user-configurable options without closing the Spectra Display Options
dialog, click on Apply. You can see the effect of the changes in the Spectra Display
window and modify them if desired.
-or-
If you are satisfied with the user-configurable options, click on OK to apply the changes
and close the dialog.
Smoothing: This option default is enabled to smooth the displayed spectra. Analytical values are
not affected. To disable this option, click to uncheck if you do not want smoothing.
Display at End: Check this option to display spectra simultaneously after all spectra are acquired.
2. Open the method that was used to generate the data. If you are not sure which method
was used, select Import from Results Library... in the Method button drop down,
then select the results data set.
3. In the Examine Spectra/MSF window, click on the name of the sample in the Samples
list to designate the active spectrum on the graphics display.
4. Drag the vertical cursor to the point of maximum intensity on the peak. The peak
maximum can be determined by observing the value in the Intensity column on the right
side of the window. The Wavelength display shows the cursor position.
5. In the Method menu, select Set Peak Wavelength.
The Wavelength display shows the chosen wavelength, and the peak wavelength symbol
is repositioned to align with the cursor.
6. In the Method menu, select Update Method Parameters...
The Update Method Parameters dialog appears. The current wavelength from the method
and the revised wavelength are shown.
7. Be sure a check mark appears next to Peak Wavelength, then select one of the following:
Update: Click on the Update button to update the method according to the revised
wavelength and any other selections you have made in this dialog. However, the method
changes will not be saved to disk.
Update and Save Method: Click on the Update and Save Method button to modify
the method according to the revised wavelength and any other selections you have made
in this dialog and save the method to disk.
8. You can view the change in the Method Editor on the Spectrometer: Define Elements page.
Tip: The analyte name specified in the method usually contains the reference wavelength (for example
As193.696), but can be renamed if desired.
To set a background correction point, choose Add Background Point from the Method menu in
the Examine/MSF window.
Tip 1: When the standards and samples are not matrix matched, it is considered good practice to use at
least a one-point background correction.
Tip 2: For any type of sloping background, use a two-point or Automatic background correction, and
select an alternate wavelength for the element whenever it is possible.
Examine Spectra/MSF/Transient Peaks Window . 265
Note: A red BGC point located at either end of the X axis indicates that the background offset in the
method is outside of the wavelength range shown in Examine. To reposition the BGC point within
the x axis, simply drag it with the mouse cursor. The color returns to green.
6. For a second BGC point repeat step 3-5, otherwise skip to step 7.
You may only select up to two BGC points per spectrum.
Note: To remove a BGC point, drag it to any position outside of the graphic display.
9. Click on the Update button to enter the new BGC points into the Method.
Note: Save the M ethod if you wish to save the updated BGC offset value(s) and correction type (i.e.,
1-Point, 2-Point or None).
Update
Click on the Update button to modify the method according to the selections you have
made in this dialog. However, the method changes will not be saved to disk. If you have
selected that you want to update the method to a new peak wavelength, be sure to select
the check box for Peak Wavelength, then click on Update.
The first column lists the wavelengths in the spectral measurement range for the analyte, Cd 228.802. The
number of wavelengths will depend on how the peak was processed as defined by the method parameters
(peak algorithm, points/peak, and, on simultaneous ICP spectrometers, whether signal profiling was used).
The remaining columns list the intensities for each data point in counts per second (cps). By using the
spreadsheet program to graph the following data points, you can re-create the peaks from the Examine
Spectra/MSF window.
Fill in the appropriate choices in the Export Spectra dialog:
• Format: Choose the column format you wish to use for displaying the wavelength data
for each sample. If all samples share the same wavelengths, select the option for Single
Wavelength Column, and the first column in the resulting spreadsheet will display the
wavelengths in the spectral measurement range as shown above. If one or more of the
samples uses a different set of wavelengths, select the option for Wavelength Column for
Each Sample, and the wavelength column in the spreadsheet will be repeated for each
sample.
• Analytes: Choose to export data for the analyte currently displayed in the Examine
window, or choose all analytes.
• Auto BGC: Choose to Export Auto BGC information or not to export any by selecting
None.
268 . Syngistix™ Software Guide
• Replicates: Choose to include data from the first or last replicate, the average (mean)
values, or all replicates.
• Data Delimited by: Choose the delimit character preferred by your spreadsheet or
database program. Columns of data can be separated by commas, tabs, or semicolons.
• File name: Select a name for the export file. Choose the same name as the data set or
create a different name.
• Extension: Choose the extension preferred by your spreadsheet or database program.
• Directory: Use the default Reports directory or browse to locate the directory where you
want to save the exported file.
Printing Spectra
You can print the spectra that are shown in the Spectra Display or Examine Spectra windows. To
adjust the printout colors, right click on the spectra and select Display Option from the popup
menu. Change the colors in the Display Options dialog. If the printer color selections have been
modified, and you wish to return to the default colors, click on Printer under the default color
settings. Click OK to close the dialog.
To print spectra:
1. Click on the Spectra Display or Examine Spectra window to make it the active window.
Note that the title bar of an active window is a different color from other windows. (The
colors displayed on your screen depend on the Windows colors you have defined for your
PC.)
3. In the Print dialog that appears, check that the correct printer is shown. If you need to
select another printer, click the drop-down arrow next to the Printer Name field. Click on
the Printer name to select it. To change other setup options such as the paper size, click
on Properties.
4. Click on OK to start printing.
The Spectra Display window always uses a layout of three rows and two columns for
printouts. Changing the layout on the screen will not affect the printout. Up to six spectra
are printed on one page. When you print the Examine Spectra window, the spectra are
overlaid in one graph on the page.
Examine Spectra/MSF/Transient Peaks Window . 269
Select: To display:
The Analytes list, which lists the wavelength for each element that was selected from Go
to Analyte.
Double-click on one of the analyte names. You can then view that wavelength for all of
the sample(s) listed in the legend.
The prior element in the Analytes list (starting from the analyte that was displayed
before you clicked on this button). If you continue to press this button, you will make
analyte selections that move back up toward the top of the Analytes list. At the top
of the list, this button ceases to function. Then, you can press the Next button or Last
button to move down the list.
The next analyte in the Analytes list (starting from the analyte that was displayed before
you clicked on this button). If you continue to press this button, you will make analyte
selections that move downward toward the bottom of the Analytes list. At the last
analyte in the list, this button ceases to function. Then, you can click on the Back button
or First button to move back up the list.
Select a Wavelength.
Note: In the Examine Transient Peaks window, time appears in place of wavelength.
270 . Syngistix™ Software Guide
You can easily allow more space for the graph or legend. To do so, position your mouse over
"splitter bar" that separates the left and right panes. Your cursor changes to a double-headed
arrow. Drag left or right to increase the size of a pane. (If your cursor does not change to a
double-headed arrow, you must disable the "auto-position splitter" option in the Examine Display
Options dialog.)
Note: The Examine MSF window is used to create the MSF model. To view the results of using MSF in an
analysis, you must open the Results Display and the Spectral Display windows. The Results Display
window lists the analytical results and indicates that the sample was processed by MSF (as
applicable, the .msf file name will be listed for each analyte in the sample). The Spectra Display
window shows both the uncorrected data and the MSF-corrected analyte data.
At the top of the graph there is a drop-down list to select which replicate mode is displayed. There are
four replicate modes: Average Replicate, First Replicate, Last Replicate, and All Replicates.
To allow more space for the legend or graph.
1. By default, the Auto Position Splitter Bar is checked in the Examine Transient Peaks
Options Dialog. This causes the system to automatically position the splitter bar, which
separates the graph from the legend, so that the legend is exactly wide enough to display
the text it contains. You can easily allow more space for the graph or legend.
272 . Syngistix™ Software Guide
2. First uncheck the Auto Position Splitter Bar check box in the Examine Transient Peaks
Options Dialog, then position your mouse over "splitter bar" that separates the left and
right panes. Your cursor changes to a double-headed arrow.
3. Drag left or right to increase the size of a pane. (If your cursor does not change to a
double-headed arrow, you must disable the "auto-position splitter" option in the Examine
Display Options dialog.)
Note: You can choose Printer colors in this dialog and then print the graph display in the Examine
Transient Peaks window as follows:
1. Right-click on the Examine Transient Peaks window and select Display Options from the
popup menu.
2. Select the Window tab to Select colors for the following items:
• Axes and Label
• Graph Title
• Analyte Mode Background
• Overlay Mode Background
• Read Delay and Read End Marks
• Time Cursor
• Axis Grid Divisions
• Active Signal Points
• Peak Maximum Mark
3. Click on the OK button to apply your choices.
You can always return to the default settings by clicking on the Defaults button.
Examine Spectra/MSF/Transient Peaks Window . 273
Note 1: MSF is not suitable where there is complete overlap of analyte and interferent (In that case, use
the Inter Element Correction (IEC). For all other types of spectral overlap, MSF is a powerful
technique that can be used to improve detection limits and precision.
Note 2: Even when there are no interferences, you can use MSF's ability to improve detection limits and
precision. (Simply create a two-component model that is composed of just the blank spectra and
the analyte spectra.) MSF is beneficial when:
MSF can automatically correct for the background so there is no need to select BGC points.
MSF uses all of the information about the peak so there is no need to select peak wavelength.
Note 3: MSF may be used along with internal standardization to further improve precision, which may be
especially important for measuring analytes in a complex matrix.
Examine Spectra/MSF/Transient Peaks Window . 275
Steps to Using M SF
An overview of how to perform Multicomponent Spectral Fitting is shown below, along with
information about how the software uses input data to calculate analyte concentration:
Type of Interference
Cause
Simple Background Shift
A high concentration of the interfering
A shift in background that is essentially constant over a analyte may emit a continuum of
given range. The background may shift either up or down. radiation in the given wavelength range
Remedy
Set a background correction point
somewhere near, but not falling on, the
profile of the analyte you are measuring.
Or select a different wavelength that is
not affected by the interferent.
Use I EC if...
You expect direct spectral overlaps.
You are taking data for use by an organization that requires Interelement Correction.
Use M SF if...
You want better interference correction, better detection limits, and better precision than are
normally obtained with IEC.
Differences
IEC MSF
Model created and IEC Model Builder window Examine MSF window
edited
Model stored IEC file MSF file
Model used in the Overlap Correction set to IEC Processing mode is set to MSF
method and IEC table name selected and MSF table name selected
in method in method
Restrictions on use You must use the same You must use the same
resolution, profiling, resolution and profiling
background correction points, settings for data collection as
and plasma parameter entries for end use.
for IEC data collection as for
end use.
282 . Syngistix™ Software Guide
Using I EC
Here is a summary of how to use the IEC model.
• Open the IEC Model Builder from the Tools menu
• Create and save the model (the .IEC file)
• Specify the IEC file in the method and save the method
• Analyze your samples or reprocess your data
N otes:
You should have the same Resolution setting, background correction points, and plasma
parameter entries for IEC data collection as for the analysis you want to correct. If you
change any of these parameters in the method, you should recreate IEC factors.
• If you have some elements for which you want to create IEC factors for multiple
wavelengths, refer to Multiple Wavelengths per Element.
• If you do not follow the procedures in Multiple Wavelengths per Element, you will get
errors if you try to collect IEC data for any element with more than one wavelength
in the method.
Inter-Element Correction . 283
Note: Before you set up the IEC model, run an analysis as you normally would and save the data.
The samples in the selected results data set are checked against samples in the IEC
model.
If the new results data set does not contain samples that are in the current IEC
model, a message appears informing you that samples are missing.
If the new results data set contains the same samples as in the IEC model, the new
results set is checked for duplicate sample IDs. If duplicate sample IDs exist, you are
given an opportunity to choose one sample from each group of duplicates.
Samples from the new result data set are checked if they contain analytes that are
part of the current IEC model. A message appears that describes each sample along
with its missing analytes.
Note: If this file has been modified but not saved, the file name in the dialog header will have an
asterisk ( * ) displayed to the right of the name. Once the file is saved, the asterisk will be
removed.
1. If you modified the IEC factors and want to save the changes, from the IEC drop-
down menu, click on Save.
2. If you modified the IEC factors and want to save the changes but also retain the
original file, from the IEC drop-down menu, click on Save As.
3. To save the information as a text file, from the IEC drop-down menu, click on Save
IEC Factors As Text.
Set Up Page
Use this page to select the Results Data Set containing the data to be used in determining
the factors. Enter comments in the Remarks field.
7. Click on OK.
After you have selected a data set, the file name appears in the Results Data Set field. The
Method Used to Collect Data field is automatically filled in.
Remarks: Use this entry field to type your comments regarding the IEC table.
Note: You may choose to skip this page and simply set low factors to zero after calculation using
the Calculate Factors page.
To select noncontiguous entries, click on an entry, then press the Control key and click on
additional entries.
Once your entries are selected, right click. When the pop-up Edit menu appears, click on
Column fill... and the Minimum Concentration Column Fill dialog will appear. You can also
display the Minimum Concentration Column Fill dialog by right clicking and selecting Column
fill....
Units: The units are the standard units, not the sample units.
Using Correction Limits: The correction limits are applied automatically and are used
during IEC factor creation and during sample analysis.
During IEC factor creation:
If an apparent analyte concentration (concentration measured at the analyte line, but due to
the interferent instead of the analyte) is greater than or equal to the analyte's correction
limit, an IEC factor for the analyte/interferent pair is calculated and entered into the IEC
factors table.
If an apparent analyte concentration is less than the correction limit, the IEC factor entered
into the IEC table for the analyte/interferent pair is zero. This is because the effect of the
interferent on the analyte was not sufficient to warrant a correction.
During sample analysis:
If an apparent analyte concentration is greater than or equal to the correction limit, the
software then applies the IEC factor to the analyte concentration and a final result is
calculated and appears in the Results Display window.
If an apparent analyte concentration calculated by applying IEC is less than the correction
limit, correction for this analyte/interferent pair is not performed. This is because the effect
of the interferent on the analyte was not sufficient to warrant a correction.
For an example of how factors are calculated, see Interelement Correction Model Builder:
Summarize Factors Page.
288 . Syngistix™ Software Guide
Note: Any errors encountered are displayed in the IEC Factors column. Error types are:
I EC Factors
Analytes: These are analytes from the method used to create the IEC table.
Interferent Reference Element: These are the names for the elements whose signals
may be interfering with the analyte signal. Each analysis element is also a potential
Interferent Reference Element.
For a given analyte, you cannot have IEC factors for more than one Reference Element per
interfering element. For example, if multiple Fe lines are used in an analysis and the analyst
needs to correct for Fe interference on an analyte line, only one of the Fe lines (i.e.
Reference Elements) can have a non-zero IEC factor in the row for that analyte.
Double-click on an Interferent Reference Element IEC factor to display the User Entered IEC
Factors dialog, where you can choose Automatic Calculation or Manually Set Factors.
Note: You can also enter a factor manually into the spreadsheet: Click on the entry and type the
new factor.
290 . Syngistix™ Software Guide
Show: Click the radio button to either Show All Analytes and all factors, even the ones
that are zero; or Only Non-zero Factors, which limits the display to only those analytes
and interfering elements where at least one value in every row and column is not zero.
Update Method: After you save the IEC file (File/Save command), click the Update
Method button to update the method in the Method Editor. When you click Update Method,
the name of the IEC file is entered in the Method Editor, Process Page, Spectral Corrections
page of the active method. The Interference Correction on all analytes with nonzero factors
will be set to IEC. IEC is automatically selected to perform Overlap Correction for analytes
with nonzero factors.
Print Factors: Click the Print Factors button to print the table of factors as currently
displayed. Print the complete table showing all analytes, or the table that contains only
analytes and interfering elements where each row and column contains at least one nonzero
IEC factor. Select the radio button to print in either Portrait (vertical) or Landscape
(horizontal)
How Factors are Calculated: The value of each factor is equal to the apparent analyte
concentration divided by the interferent concentration. The apparent analyte concentration is
the concentration measured at the analyte line, but due to the interferent instead of the
analyte.
When you analyze samples, the software multiplies the interferent concentration by the IEC
factor. It then subtracts this product from the measured analyte concentration to result in
the corrected analyte concentration.
For example, suppose you are determining As and you know that Fe is creating an
interference. You find that:
Multiplying:
Note: If you do not use these guidelines, you will get errors if you try to collect or use IEC data for
any element with more than one wavelength in the method.
Inter-Element Correction . 291
• For a given analyte, you cannot have IEC factors for more than one Reference
Element per interfering element.
For example, if multiple Fe lines are used in an analysis and the analyst needs to correct for
Fe interference on an analyte line, only one of the Fe lines (i.e. Reference Elements) can
have a non-zero IEC factor in the row for that analyte.
• Also, it is important when an IEC Standard for an interfering element with multiple
lines in a method is analyzed, that the other "elements" defined for the interfering
element are not analyzed as analytes. Otherwise, you would be making a correction
for an element on itself.
For example, you would be correcting for the interference of Fe on Fe.
• To ensure that only one Reference Element per interfering element has IEC factors
associated with a given analyte, it is best to analyze only one IEC Standard per
interfering element. To avoid the situation where an element is corrected for
interference upon itself, you can disable data collection for those elements by using
the Enable/Disable Elements function. See the Analysis Menu.
Ex am ple 1
As an example, suppose you have a method that contains three Fe lines named Fe1, Fe2,
and Fe3. For the simplest case, we will use Fe1 as the Reference Element for all IEC
corrections. To create IEC factors for Fe interference correction:
1. Calibrate using the method as usual using the Calib page.
2. When ready to analyze the Fe IEC Standard on the Analyze page:
a. Select Fe1 as the Reference Element.
b. In the Analysis menu, open the Enable/Disable function and disable Fe2 and Fe3.
c. Analyze the Fe IEC Standard.
Note: Remember to re-enable Fe2 and Fe3 before measuring IEC Standards for other elements.
Ex am ple 2
In a more complex example, suppose that you are using the same method containing three
Fe lines, but you want to use Fe1 as the Reference Element for correction of Fe on As and
Fe2 for correction of Fe on Cr. You may want to do a correction of this sort so that you can
match an interferent atom line with an analyte atom line and interferent ion line with an
analyte ion line to improve the quality of the interference correction. To create the Fe IEC
factors for this situation:
1. Calibrate as usual.
2. To create the factor for correction of Fe on As,
a. Select Fe1 as the Reference Element.
b. Disable Fe2, Fe3, and Cr.
c. Analyze the Fe IEC Standard.
d. Select Fe2 as the next Reference Element.
e. Re-enable Fe2 and Cr and disable Fe1 and As (Fe3 should still be disabled).
f. Analyze the Fe IEC Standard.
Remember to enable the disabled elements before measuring other IEC Standards.
292 . Syngistix™ Software Guide
Calibration and Calculations
294 . Syngistix™ Software Guide
Calibration
• Linear Calibration
• Linear Forced through Zero
• Linear Bracketing Calibration
• Non-Linear Calibration
• Non-Linear Bracketing Algorithm
• Correlation Coefficient
• Weighted Linear Calibration
• Method of Additions, Sample Intercept
• Method of Additions, Calculated Intercept
• Method of Additions Calibrate
Calculations
• Standard Deviation and Precision
• Reslope
• Internal Standardization
Calibration and Calculations . 295
Edit Calibration
You use the Edit Calibration window to recalculate the calibration curve for the selected
element or elements using Include and Reanalyze options. When you first display this
window, the Include option is selected for each calibration standard.
Note: In this window, you can make changes to the Calibration Equation. These changes will be
saved in the Method Editor.
First, Previous, Next, Last Buttons Use these buttons to change the
currently displayed analyte.
Calibration Display: The graphical display of the analyte calibration showing the standard
point residual lines, excluded points (using the check boxes in the Include column of the
table to the right of this display.
Slope: This is the slope of the calibration curve. For a nonlinear curve, this is the slope at
zero concentration.
Intercept: This is the zero concentration, which is the value of the point at which the
calibration curve crosses the Y-axis.
Correlation Coefficient: This indicates how well the data fit the calibration curve. In
general, the better the fit, the larger the correlation coefficient. A value of 1.0 indicates a
perfect fit.
Last Sample Concentration: This is the concentration of the last sample analyzed in the
calibration units. A value will only be given for unknown samples.
Calibration Table:
Std#: The number of each standard as defined in the current method.
Include: Click in the check box to select each calibration standard that you want the
system to use when it recalculates the calibration curve. With multi-element instruments, this
option affects only the calibration curve for the selected element.
296 . Syngistix™ Software Guide
Note: Reanalyzing cannot be done with MSA (Method of Additions), if the curve was opened via
Recall Calibration. In this case, the Reanalyze check boxes are disabled and cannot be
selected.
Calibration Equation: This is the calibration equation selected on the Calibration page of
the Method Editor window.
Reanalyze Standards: This shows the number of selected standards to be reanalyzed.
Reanalyze: The system reanalyze the calibration standards and recalculates the calibration
curve using all the options that you have selected.
To edit a calibration curve:
1. Display the Edit Calibration dialog.
2. Select a desired Analyte from the drop-down menu to display the calibration
curve you want to change.
3. To include a standard listed in the table, click the corresponding check box in the
Include column.
4. To reanalyze one or more standards, click the check box of the desired standard in
the Reanalyze column.
The selected standard appears in the Reanalyze standards table. You can also select
to Reanalyze for all analytes or Reanalyze for selected analytes only.
5. To recalculate a new calibration curve using a different equation, select a different
Calibration equation from the drop-down list.
6. Press the Reanalyze button.
To edit calibration display options:
Right-click on the graph and select Display Options. The Calibration Display
Options window appears. Select colors for the screen and printer.
To Delete a Calibration:
On the Results tab, in the Calibration group, click on New Calibration.
Calibration and Calculations . 297
This calibration curve is established by assuming that the relationship between concentration
(the X values) and intensity (the Y values) is linear and that the following equation describes
this relationship:
Y = MX + B
where:
X = concentration
Y = intensity
M = slope of the calibration curve
B = y-axis intercept
Given two or more data points, the values for M and B are calculated using the following
equations [1, 2].
n = number of standards (includes the blank)
In this equation, the intensity of the blank is subtracted from all solutions and included in the
calculation of the calibration curve.
[1]
[2]
298 . Syngistix™ Software Guide
An example of this calculation is described below. The Syngistix Report shows the following
information for Ag: 328.068:
Where:
The intensity of the blank is subtracted from the Net Intensity to get the Corrected Intensity
which is calculated as:
52083.0 ( 59.6)=52142.9
Then the Corrected Intensity is used to calculate the concentration as …
(52142.9-0.0)/101200=0.5
… using the equation Y=MX+B to solve for X, so X=(Y-B)/M
Please note that the numbers derived from the calculation above may differ slightly from the
intensity value displayed in the Syngistix report, because Syngistix calculates Intensity values
using additional significant figures for the Concentration value; these additional significant
figures are not displayed on the printed Syngistix report.
Calibration and Calculations . 299
This calibration curve is established by assuming that the relationship between concentration
(the X values) and intensity (the Y values) is linear and that the following equation describes
this relationship:
Y = MX
where:
X = concentration
Y = intensity
M = slope of the calibration curve
The intercept is forced to be zero.
Given 2 or more data points, the values for M are calculated using the following equation.
n = number of standards (includes the blank)
In this equation, the intensity of the blank is subtracted from all solutions and included in the
calculation of the calibration curve.
300 . Syngistix™ Software Guide
This calibration curve is established by assuming that the relationship between concentration
(the X values) and intensity (the Y values) is a curvilinear one that can be described by the
following polynomial equation:
X = concentration
Y = intensity
A = curvature
B = slope
C = y-axis intercept
Given 3 or more data points, the values for A, B and C are calculated using the following
equations [1, 2, 3].
n = number of standards (includes the blank)
In this equation, the intensity of the blank is subtracted from all solutions and included in the
calculation of the calibration curve.
[1]
[2]
[3]
Where:
Calibration and Calculations . 301
302 . Syngistix™ Software Guide
This calibration curve is established by assuming that the relationship between concentration
(the X values) and intensity (the Y values) is a curvilinear one that can be described by the
following polynomial equation:
where:
X = concentration
Y = intensity
A = curvature
B = slope
C = y-axis intercept
Given 3 or more data points, the values for A, B and C are calculated using the following
equations [1, 2, 3].
n = number of standards (includes the blank)
In this equation, the blank is subtracted from all solutions and included in the calculation of
the calibration curve.
The use of a blank is optional. If a blank is not used, a zero intensity is assumed. In this
equation, the intensity of the blank is subtracted from all solutions, but is not included in the
calculation of the calibration curve.
[1]
[2]
Calibration and Calculations . 303
[3]
Where:
304 . Syngistix™ Software Guide
Correlation Coefficient
Correlation coefficients are calculated in Syngistix using three different formulas, based on
the current calibration equation.
Linear Calculated Intercept / Linear Bracketing
Where:
X = concentration
Y = intensity
n = number of standards+1
Based only on concentration (intensity) points, not the calculated curve.
Coefficient may be 1.0 even if points are not on the curve.
For Linear Calculated Intercept, the blank (0,0) point is included, which increases the number
of standards (n) by 1.
Where:
X = concentration
Y = intensity
n = number of standards
Based only on concentration (intensity) points, not the calculated curve
Coefficient may be 1.0 even if points are not on the curve
Nonlinear (Calculated Intercept / Zero Intercept / Bracketing)
Where:
X = concentration (entered by user)
Y = concentration (measured from calibration curve)
Calibration and Calculations . 305
n = number of standards
Based on actual and measured concentrations (the delta between the user-entered value and
the calculated curve).
Will work for linear or non-linear curves
Coefficient will be 1.0 only if all points are on the curve.
For Nonlinear Calculated Intercept, the blank (0,0) point is included, which increases the
number of standards (n) by 1.
306 . Syngistix™ Software Guide
Where:
The equation used to calculate precision or the Relative Standard Deviation (RSD) is:
Calibration and Calculations . 307
When working at low level concentrations it provides an alternative calibration scheme that
weighs the low standards to a greater degree.
Determine the slope, intercept, and correlation coefficient for the equation:
where x is the measured net corrected intensity (blank subtracted). The weights are applied
by multiplying the intensity by the weighting factor for each standard. In this calibration the
weighting factor is the reciprocal of the square of the user entered concentration value for
each standard.
Where:
x is the Concentration value of the standard
y is the measured intensity of the standard
n is the number of standards
i is the index for the standards
b0 is the intercept
b1 is the slope
C is the correlation coefficient
308 . Syngistix™ Software Guide
Calibration and Calculations . 309
Use the analyte addition technique when the matrix causes an interference that varies from
sample to sample.
The calibration curve is forced to go through the point defined by the sample with no
addition added, and in the other the sample with no addition is treated as just another point
by the least squares routine.
The equation used for the sample intercept option is:
C is the concentration added to an aliquot of sample and I is the difference between the
intensity for the aliquot with added standard and the intensity measured for the sample. The
final sample concentration is calculated by multiplying the slope (-K1) times the intensity of
the sample.
310 . Syngistix™ Software Guide
A least squares technique is used to determine the K1 coefficient when two or more
standards are used for calibration. This calibration curve is not forced to go through the point
defined by the unspiked sample and the intercept with the intensity axis is calculated.
The equation used for the calculated intercept option is:
The sample with no addition is treated as just another point by the least squares routine that
determines the K1 and K2 coefficients.
Calibration and Calculations . 311
The system uses method of additions, with the zero intercept equation option for the first
sample then analyzes subsequent samples using the calibration curve generated for the first
sample. This is appropriate when the matrix causes an interference that is the same for all
the samples.
This calibration curve is forced to go through the point defined by the unspiked sample.
312 . Syngistix™ Software Guide
concentration of each standard in each spiked sample (A1, A2, etc.) is set to the
concentration added to each spiked sample.
You need to specify the concentration of standard in each spiked sample (A1 and A2) on the
Calibration: Calibration Units and Standard Concentrations page of the Method Editor. The
concentration of each standard in each spiked sample (A1 and A2) is set to the concentration
that is added to each spiked sample. The values of 10 and 20 used in this example (for A1
and A2, respectively) were obtained using the following formula:
Value = Vol. of stock std. X Conc. Of stock std.
Vol. of sample
Note: If you are not using a sample information file, you can enter a Sample ID for each sample in
the Manual Analysis Control window. You can use the assigned ID or assign a name to each
sample. If you want to enter an individual ID, type a name, any combination of letters and
numbers, up to 25 characters.
each standard in each spiked sample (A1, A2, etc.) is set to the concentration added
to each spiked sample.
A
Analyte. The element whose concentration is determined in an analysis.
Array detector. A silicon chip that is manufactured with a one or two-dimensional array of
photosensitive material on its surface. The photons that are absorbed by the units (pixels) of
the array are converted to electrons which are collected and read out. Examples include
Photodiode Arrays (PDAs), Charge-coupled Devices (CCDs), Charge-injection devices (CIDs)
and Segmented-array Charge-coupled Devices (SCDs).
Aspiration. A high-speed gas flow is directed across an open tube to draw solution into the
nebulizer.
Auxiliary flow. The flow of argon gas that is contained between the intermediate and the
injector tubes of the ICP torch.
Automatic Background Correction. Automatic Background Correction is the default
setting for Spectral Corrections in all new methods. Methods created before version 5.1 will
remain as previously saved, but will have the added option of setting the background
correction to automatic in the Method Editor.
Automatic background correction (ABGC) uses a propriety PerkinElmer algorithm that
dynamically creates a background correction spectrum for each ICP replicate and/or average
spectrum with no user interaction required. The algorithm takes the points in the sample
spectrum itself and calculates the best fit of background spectrum.
The Automatic Background Correction spectrum is then subtracted from the original sample
spectrum to get the background corrected spectrum.
B
Background correction. Process of correcting the intensity recorded for a particular
wavelength for intensity due to the ICP continuum background and other spectral
interferences. This is normally done by choosing one or two points at one or both sides of
the peak you want to correct. Points can be chosen manually. The software then measures
the intensity at these points, interpolates an intensity at the peak wavelength, and then
subtracts that intensity from the intensity recorded at the peak.
BEC test. Background Equivalent Concentration test. A test of instrument sensitivity. The
concentration of a solution whose intensity is equivalent to the intensity of the background at
the same wavelength is determined. The lower the concentration of this solution, the more
sensitive the instrument for that element.
Blank (solution). A solution that contains none (or rather, an undetectable amount) of the
analyte you are interested in. Used for a zero point in calibration.
C
Calibration curve. The plot or equation showing intensity versus concentration for an
analyte. Once this is established, the concentration of any solution containing this analyte
within the concentration range of the calibration can be found.
Calibration equation. Mathematical function used to convert a sample's measured
emission intensity into a concentration reading. See also Curve Type.
CCD. Charge-coupled Device. A two-dimensional array detector that uses a charge-coupled
readout of the photoelectrons generated by light absorption. This type of detector is used in
PerkinElmer Scanning CCD ICP spectrometers. See also Array detector, SCD.
Correlation coefficient. Indicates the quality of the fit between the calibration curve and
the points it is fitting. A value of 1.000 indicates a perfect fit.
Glossary
Curve type. Describes the calibration curve made using a particular calibration equation.
Using different curve types for the same standard and blank measurements may give
different analytical results.
CV test. Coefficient of Variation test. See Relative Standard Deviation (RSD).
D
Default settings. The instrument software contains standard settings which are the most
generally used settings. There are default settings for aqueous and organic analyses that are
available to use as a starting point when creating a new method.
Detection limit. The lowest concentration of an analyte whose presence can be determined
with a specified degree of certainty. Often defined as the concentration of an analyte that
results in signal intensity that is three times (or twice) the standard deviation of the
background intensity at the wavelength measured.
Detector. A photosensitive device that absorbs photons and converts them into electrons
with a certain efficiency. These photoelectrons can be measured to indicate the intensity of
the incoming light, that is, the number of photons from the emission source. See also Array
detector, CCD, and SCD.
Difference spectrum. Spectrum that results from subtracting one spectrum from another.
E
Echelle grating. Coarsely ruled diffraction grating used in multiple orders to achieve high
spectral resolution.
Excitation characteristics. The amount of energy required to promote an electron to a
higher energy level in an atom or ion. This excited state is necessary for the atom or ion to
emit light. Different elements have different excitation characteristics.
F
Firmware. Programmable silicon chips that form an interface between the computer
software and the instrument hardware that it controls. Firmware has a restricted set of
commands but operates extremely fast, thus allowing the software to be simpler and speed
up instrument response.
FIAS. Abbreviated for Flow Injection Analysis System
G
GPIB. General-Purpose Interface Bus. A commonly used protocol (agreement) on how
computers and electronic devices should communicate. The computer uses a GPIB card to
allow it to communicate with the instrument firmware.
I
IEC. See Interelement Correction.
IEEE-488. Common interface protocol for communications between computers and other
electrical devices.
Integration time. The time for which the detector absorbs photons from the plasma before
a signal is read out. The integration time multiplied by the number of reads specified equals
the read time.
Interelement Correction (IEC). A spectral interference correction technique in which
emission contributions from interfering elements that emit at the analyte wavelength are
subtracted from the apparent analyte emission after measuring the interfering element at
another wavelength.
322 . Syngistix™ Software Guide
Intercept. Where two lines meet. Commonly used in spectroscopy in calibration work, for
example, the y-intercept, meaning the point where the calibration curve cuts the x= 0 axis of
the calibration plot.
Interference. Anything that causes the analyte signal in a sample to differ from the analyte
signal in a calibration solution at the same concentration. See also Spectral interference.
Internal reference. IUPAC name for internal standard.
Internal standard. A nonanalyte element, present in all standards, blanks, and samples,
that is used to correct for physical or matrix interferences in an analysis.
L
Linear fit. Type of calibration curve where a straight line is drawn through the standard and
blank emission/concentration values.
M
Matrix. The components of the sample other than the elements of interest. The matrix can
substantially change results obtained, through spectral interference or viscosity change.
Mercury lamp. A lamp inside PerkinElmer simultaneous ICP spectrometers that emits light
at a mercury wavelength. This is periodically used to return the instrument to the current
wavelength calibration.
Method. Controls instrument settings and how the instrument acquires and processes data
in an analysis.
MRU. Most recently Used. Displays the last few most recently used Methods, etc.
MSF. See Multicomponent Spectral Fitting.
Multicomponent Spectral Fitting (MSF). A processing mode that distinguishes analyte
spectra from interfering spectra by the use of stored mathematical models. It uses a multiple
linear regression technique to fit the models created to unknown spectra during an analysis.
Since only the peak shapes need to remain constant, typically, the models are independent
of concentration, plasma conditions, and matrix effects.
N
Nebulizer Flow. The flow of argon gas that enters the nebulizer and carries the sample in
the form of an aerosol into the plasma.
Neon Correction. A neon reference spectrum is measured for use in wavelength correction
on PerkinElmer Scanning CCD ICP spectrometers.
O
Optimizing. The process of determining the best conditions and settings for an analysis.
Outer Flow. IUPAC term for plasma flow.
P
Peak algorithm. The way in which the emission data from the spectrometer is converted
into emission counts. This can be done in three ways: (1) by searching for a peak and
estimating its height (Peak height processing); (2) by summing the output of several detector
Glossary
pixels (Peak area processing); or (3) by treating the output mathematically and relating it to
existing spectral models (Multicomponent Spectral Fit processing).
Peak area processing. A processing mode that sums the intensities recorded by specified
pixels on a given subarray for an element.
Peak height processing. A mode of processing emission data where the highest intensity
points are searched for, and then an algorithm is applied to approximate the peak height.
See also Area processing and Multicomponent Spectral Fitting.
Pixel. Photosensitive unit of an array detector whose output can be read individually.
Polychromator. A type of spectrometer that can detect and process data for two or more
wavelengths at the same time.
Pre-shot. A quick "snapshot" of the plasma emission which is made by the spectrometer
when Auto Integration is selected. This is used to determine optimum integration times.
Precision. A measure of how reproducible a set of measurements is. Commonly used
statistical measurements are standard deviation (SD) and relative standard deviation (RSD),
also called coefficient of variation (CV).
R
Read time. The amount of time per replicate for which the detector measures light from the
plasma for the current sample. The total read time equals the integration time multiplied by
the number of integrations specified.
Relative Standard Deviation (RSD). The standard deviation of a group of measurements
divided by the mean of those measurements. A test used to measure relative precision for a
group of measurements. Often expressed as a percent. Also known as Coefficient of
Variation (CV) test.
Replicate. A sample can have one or more replicates, meaning that there will be repetitive
measurements taken.
Residual Error. The amount the calibration standard deviates from the entered concentration
as a percent. Calculated as: ((calConc - enteredConc) / enteredConc) * 100.00
Reslope. When there are small changes in instrumental conditions, the reslope feature of
the software allows you to compensate by making small corrections to the calibration curve
using a single calibration standard.
Resolution. The measure of a spectrometer's ability to separate adjacent wavelengths. The
High setting for resolution maximizes the resolving power on PerkinElmer simultaneous ICP
spectrometers.
RF Power. The amount of energy per unit time transmitted from the RF generator to the
ICP discharge. Measured in watts.
S
Sample uptake rate. IUPAC term for sample flow rate.
Scanning CCD ICP Spectrometer. A spectrometer that detects and processes data for
one wavelength at a time.
Simultaneous ICP Spectrometer. A spectrometer that detects and processes data for two
or more wavelengths at the same time.
SCD. Segmented-array Charge-coupled device Detector. A specialized type of array detector
(developed for and used in PerkinElmer simultaneous ICP spectrometers) that has groups of
photosensitive pixels, called subarrays, on the detector surface where important atomic
324 . Syngistix™ Software Guide
emission lines appear. The SCD uses charge-coupled readout like a CCD, but the subarrays
can be individually addressed. See also Array Detector, Detector, CCD.
Slit Steps. The number of positions used by the spectrometer entrance slit during data
collection for each replicate on simultaneous ICP spectrometers. The slit can be moved under
software control. When the spectral profiling is set to off, the spectrometer uses one slit step
(entrance slit position); when spectral profiling is on, the spectrometer uses four.
Shutter. A mechanical device used to block the plasma emission from entering the
spectrometer.
Spectral interference. An interference caused by the emission from elements or
compounds other than those of interest.
Spectral profiling. On PerkinElmer simultaneous ICP spectrometers, the spectrometer
entrance slit is adjusted by ¼ pixel steps during data collection, thus moving the slit image
across the detector sub-arrays. This increases the data density across the spectral peaks and
produces smoothed spectral displays.
Split-pixel. Reading a detector array so that information is taken from each half-pixel rather
than from each pixel.
Standard. A solution with accurately known concentrations of the elements to be
determined in an analysis. Two or more standards are used to make a calibration curve.
Standard deviation. A statistical definition of the variation in a group of similar
measurements.
Structured background. Spectral interference that is non-random, thereby altering
analytical results for nearby analyte lines.
Subarray. On PerkinElmer simultaneous ICP spectrometers, this is a group of pixels on an
SCD which are positioned to measure a small, specific wavelength range.
T-Z
Weighted linear fit. A curve type where the importance given to a calibration point in the
fitting process (the weighting) is directly related to the concentration of the standard
measured for that point.
I ndex
Automated Analysis Control
A overview ........................................... 187
Automated Analysis Control command
A/S Location entry .................................. 112 Tools menu ......................................... 20
active autosampler
method ............................................... 68 setting up............................................ 52
adding rows .......................................... 153 Autosampler command
Additional Message entry.................. 134, 136 Analysis menu...................................... 21
After Initial Calib entry ............................ 133 Autosampler Configuration dialog ............. 215
After Recalibration entry.......................... 133 Autosampler Loading List ........................ 256
algorithms ... 292, 295, 297, 298, 300, 302, 304 Autosampler Location Column Fill dialog .... 167
Aliquot Volume Column Fill dialog ............. 172 Autosampler Location entry ..................... 161
Aliquot Volume entry .............................. 162 autosampler model
An Overview of MSF Function................... 273 selecting ........................................... 215
analyses Autosampler page .................................... 95
performing Method Editor ...................................... 95
overview ......................................... 44 autosampler tray
analysis control windows selecting ........................................... 215
overview ........................................... 182 Aux entry ................................................ 91
Analysis Header ..................................... 246
Analysis menu commands.......................... 21
B
analysis schedule parameters ................... 164
Analyst Name entry ................................ 161 Background Correction entry.................... 105
analyte ................................................. 268 Background Correction Point option .......... 264
displaying in Examine Spectra/MSF ....... 268 Batch ID entry ....................................... 161
standard concentrations ...................... 116 BGC1 entry............................................ 105
Analyte information field................... 116, 127 BGC2 entry............................................ 105
Analytical Header ................................... 246 Buttons
Analytical Header command Toolbar ............................................... 10
Analysis menu...................................... 21
analytical sequence ................................ 187 C
Analyze QCs Before Column Fill dialog ....... 175
Analyze QCs Before entry ........................ 164 Calculate Factors for IEC ......................... 285
analyzing samples Calculate Limits button............................ 132
overview ............................................. 44 Calculate Limits dialog ............................ 127
archiving calculation
libraries.................................................8 disk storage space .............................. 200
Assign Internal Standards entries.............. 107 Calib Blank Action entry .......................... 118
Assign Internal Standards page Calib Std entry ....................................... 116
Method Editor .................................... 107 Calib Units entry .................................... 116
At End entry .......................................... 133 calibration ............................................. 172
Auto button creating new...................................... 124
Toolbar ............................................... 10 initial
Auto Dilution Factor ................................ 176 for automated analyses ................... 124
Auto Dilution Factor Column Fill ................ 176 selecting color.................................... 254
Automated Analysis command units
Analysis menu...................................... 21 editing .......................................... 116
326 . Syngistix™ Software Guide