icp software qtegra
TRANSCRIPT
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ICP SOFTWARE QTEGRA
G A M A L A . H A M I D
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Gamal A. Hamid2
Thanks
To everyone who has helped us with support,
new books, hard/soft ware And over the internet
Special thanks for Thermo
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Contents
• Introduction
• Configurator
• Qtegra
Templates
Labbooks
• Getting started
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INTRODUCTIO
N
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ICP or ICP-AES or ICP-OES
• It is a multi-element analysis technique
that will dissociate a sample into its
constituent atoms and ions and exciting
them to a higher energy level.
• Cause them to emit light at a characteristic
wavelength , which will be analyzing
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Qtegra ISDS
Qtegra is the main module of the
Thermo Scientific Qtegra Intelligent
Scientific Data Solution (ISDS) and is
used to design, start and stop the
measurements of ICP.
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Qtegra Compliance with 21 CFR Part 11
• Part 11 of Title 21 of the Code of Federal Regulations,
Electronic Records, Electronic Signatures (21 CFR Part 11)
includes the U.S. federal guidelines for storage and protection
of electronically stored data and the application of electronic
signatures.
• The new Qtegra ISDS software provides a wide range of
features which enable laboratories to operate within total
FDA compliance. These features include audit trails, support
for electronic signatures and tools for integrated data
managements.
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CONFIGURATO
R
The Configurator tool contains all
tools necessary to configure and
adjust the Qtegra ISDS framework
for your laboratory
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Contents
1. Access Control Editor
2. Experiment Configurator
3. Report Editor
4. Settings
5. Standard Editor
6. Viewer Region
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1. Access Control Editor
• Allows the Administrator and Manager to
control the access permissions by granting
or denying access to the different programs
and applications of Qtegra ISDS.
• Configurator - Access control editor -
Select an item from Virtual instruments or
Virtual evaluations - Access mode - Click
to display the list of access rights
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2. Experiment Configurator
• The Experiment configurator applet of the
Configurator tool combines instrument
sets.
• Each combination is saved as specific
Configuration for later use in the Qtegra
tool when creating a Template.
• Generally, only the Administrator and the
Manager have full access to this module
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Enabling the Drain Flow Sensor
• The Drain Flow Sensor is a unique safety
and time saving device which uses a bubble
counter to check that at least one bubble
passes from the instrument spray chamber
drain every two minutes.
• This ensures that if the sample introduction
becomes blocked/sample tubing has
detached that valuable time and gas is not
wasted by continuing the run.
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3. Report Editor
• The Report editor is a tool allows you to
create new report templates or to edit existing
templates.
• Report editor determines the layout of the
reports.
• To create a new report template
Configurator - Report editor - create a new
Report template.
Enter a Report name - Configure the layout -
save the Report template.
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4. Settings
• The Settings applet of the
Configurator tool controls default
settings,
• Configurator – Setting - Select
Logging and click Show All.
Set the Value for Misc. to True
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5. Standard Editor “ Global standards”
• The Standard Editor is a tool gives
access to the standards database.
• New standard files, and internal
standard files are created here.
• Standard Editor shows a list of
standards on the left.
• On the right the associated elements
and their concentration in the
standard solution are displayed as well
as the periodic table.
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6. Viewer Region
• The Viewer region displays a list of log files,
such as messages, errors and warnings.
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QTEGRA Qtegra ISDS is a configurable software
package for elemental analyses. It is a
true end-to-end solution for
workflow-driven analysis.
softw
are
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Contents
Qtegra user Interface
1) Dashboard Page
2) LabBooks Page
3) Templates Page
4) LabBook Query Page
5. File Manager Page
6. Help Page
7. Scheduler
8. Completed LabBooks
9. Log View
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Qtegra user Interface
• The Home Page It contains all
functions offered by Qtegra and gives
access to all existing Templates and
LabBooks.
• The pages for measurement, result
analysis, the management of files and
helpful links are also accessed via the
Home Page.
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1. Dashboard page
It shows on one page the instrument controls and main settings of the iCAP 7000.
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Interlocks
Interlocks
• Check the interlocks are all green and take
appropriate action if any are RED.
• When all interlocks are green click on the
“red ringed” Get ready icon on the
Dashboard Page.
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Plasma
• Inductively Coupled Argon Plasma using
radio frequency bands. Solid state RF
generator with power efficiency >78 %.
• Nominal Frequency: 27.12 MHz
• Plasma ignition and operation are fully
automated and pc controlled.
• Power Output: iCAP 7200 ICP-OES power is
pre-optimized at 1150 watts. iCAP 7400 ICP-
OES 750 - 1500 watts computer controlled in
steps of 25 watts. iCAP 7600 ICP-OES 750 -
1600 watts computer controlled in steps
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Get ready
• It helps to start the instrument, switches on the
plasma and waits for the instrument to warm up.
• The Get Ready icon shortly shows yellow until
the state changes to ready while the plasma is
switched on, When the warm-up starts the icon is
already green.
• After warm-up, the spectrometer optimization is
started.
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Spectrometer Optimization
• The Spectrometer Optimization function may be performed at any
time, and is a routine which ensures that the wavelengths are
correctly located on the detector.
• This routine will automatically run when the plasma is ignited.
• During this routine, the pump will stop and the nebulizer gas will
be turned off.
• NOTICE It is recommended that the Spectrometer Optimization
function is carried out prior to analysis.
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Nebulizer Optimization
• The Nebulizer Optimization optimizes the
nebulizer pressure settings for the
performance tests.
• NOTICE Standard concentric glass nebulizers
are optimized for a flow of approximately 0.7
to 1 L/min.
• Ensure that gas flows in excess of 1.0 L/min are
not used as this may result in sub-optimal
performance.
• Other nebulizers may run at higher flows.
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Performance test
• The performance checks are defined by the Sensitivity,
Relative Standard Deviation, and Detection Limit tests.
• The performance checks should be run using the
standard aqueous solutions kit.
• Once the performance checks are passed, the
instrument is ready for operation. If the performance
checks fail, check for causes and run the tests again.
• The Performance Check is followed by the Relative
Standard Deviation test and the Detection Limit.
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Passed or Failed
• When the procedure has been finished, the
display changes accordingly.
• The display shows Failed for tests that have
not been passed successfully,
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Torch Alignment
• For maximum sensitivity it is advisable to check the
alignment of the torch whenever it has been
removed and replaced in the instrument or if the
torch body or centre tube has been replaced.
• Four Alignment steps are performed.
Radial, slit=UV follow, slit=Vis,
Axial, slit=UV, and, slit=Vis.
• The 2 ppm Zinc Solution for Torch Alignment should
be made up with either an aqueous or an organic
matrix as required.
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Auto peak
• iCAP will automatically check a reference line each
time the plasma is ignited to maintain wavelength
accuracy.
• wavelengths are correctly aligned in the centre of
the sub array measurement window
• Only needs to be run whenever a new wavelength
is used for analysis or if the instrument has been
switched off for an extended period of time.
• Allow the plasma to stabilize for 10 minutes.
• Introduce the sample “Method development
standard” (high standard concentration solution of
the selected element(s).
Using the iCAP 7000 Test
Solution ( High Concentration Standard
Solution containing: 10ppm P, 5ppm K,
Ni; 1ppm Al, Mn, Cu and 0.2 ppm Zn,
Mg, Ca, Ba, 0.2% HNO3).
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Organic material
Organics Check box
To enable Auto peak to be performed with
organic standards.
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Closing Down the System
• The iCAP 7000 Series ICP-OES system can
be shut down with the Shut Down function
on the Dashboard page of Qtegra.
• The iCAP 7000 Series ICP-OES system shuts
down and the plasma switches off.
• The state of the Configuration changes to
Not Ready.
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The Post Ignition Defaults
• Post Ignition Defaults can be set in order to
immediately change start-up settings, all at
the same time.
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Changing the Configuration
• It is frequently necessary to change the
Configuration of the iCAP 7000 Series ICP-
OES instrument.
• With the Change Configuration function on
the Dashboard page of Qtegra you can
easily change the Configuration.
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Using autosampler
• If you run the tests using an autosampler, enter Wash time and Uptake time, as
well as Rack and Vial position for Multi Element Test Solution and Blank
solution.
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2. LabBooks Page
• On the LabBooks page of Qtegra,
LabBooks are created and opened.
• LabBooks are created from :
1. Blank Templates,
2. Existing Templates or from
3. Existing LabBooks .
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3. Templates Page
• The analytical workflow for sample
measurement is defined in a Template.
• select a template in recent template
• Or create a new template.
• Or open a saved template
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Template Sections
A Template contains all basic information on
analytes, Template consists of :-
• A Method Parameters section,
• A Sample Definition section,
• An Automatic Export section,
• And a Peripherals section.
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4. LabBook Query Page
• the location of the LabBooks and the
period of time measurements were done
and parse through the available results.
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5. File Manager Page
• Organize your Template and LabBook files.
• On the File Manager you can cut, copy, delete or rename your Template and
LabBook files
• The folder Performance Report gives access to the performance test results.
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6. Help Page
• provides information about Qtegra
ISDS, support and tools.
• In the Support section on the Help
page of Qtegra offers access to the
Qtegra ISDS Help.
• In the Tools section on the Help page
of Qtegra, you can customize your
Home Page settings.
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7. Scheduler
• In the Scheduler tool of Qtegra, the
measurement for a scheduled LabBook is
executed.
• The completed LabBook is automatically
deleted from the Scheduler and added to
“Completed LabBooks”
• To add a LabBook to the Scheduler
Qtegra - Open a LabBook - In the toolbar of
the LabBook, click to schedule the
LabBook.
The LabBook is added to the Scheduler
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8. Completed LabBooks
• Upon completion of a LabBook, the LabBook is automatically deleted from Scheduler and
added to the Completed LabBooks tab in Qtegra.
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9. Log View
• The Log View region of Qtegra displays a list of messages, such as errors and
warnings. By default, different types of messages are displayed.
• (The Viewer tab is also shown in “Configurator”
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A TEMPLA
TE
The analytical workflow for
sample measurement
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Content
1. Method parameters
2. Sample definition
3. Automatic export
4. Peripherals section
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Evaluation
eQuant
• Uses external element concentrations to
quantify element concentrations in an
unknown sample.
Raw Data
• Displays the acquired raw intensities which
are then used by the different evaluations.
Method Parameters
• might differ, depending on the Evaluation
selected for the Template or LabBook in
Qtegra.
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Template tool bar
• Save,
• Close or run a Template,
• Create a new LabBook or Template from the existing current Template,
• View the history of the current Template,
• Hide the Content pane,
• Auto peak,
• Time Study, show transient signal during exposure.
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1. Method Parameters
a. Analytes
b. Measure Modes
c. Acquisition Parameters
d. Intelligent Uptake and Rinse
e. Inter-Element Correction
f. Standards
g. Quantification
h. Ratios
i. Quality Control
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a. Analytes
• The analytes to be acquired during the
measurement.
• Analytes can directly be selected from the
periodic table display
• For some elements, several analytical
wavelengths are displayed in descending
order of relative intensity.
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Lines interferences
• The details of the element are displayed
with symbol, wavelength, relative
intensity, state and known interferences as
stored in the element database
• The wavelength of the analyte is displayed
in the yellow graph
• The wavelength of the interference is
displayed in the red graph
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b. Measure Modes
• Parameters are defined in order to optimize
the analysis by the radial and/or axial
configurations.
• In the axial configuration, the plasma is viewed
end-on (along the length of the plasma). That
offers greater sensitivity.
• In the radial configuration, the plasma is
viewed from the side. The radial plasma view
offers less sensitivity
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Full frame
• With the Evaluation Results Full Frames view of the LabBook in Qtegra you can identify all
the elements present.
• Method elements are shown on the right in the Elements panel.
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c. Acquisition Parameters
Analysis Mode
Normal mode is the traditional analysis mode which is per replicate.
Speed analyzes all radial/high wavelength elements for all replicates, then all axial/low
wavelength elements for all replicates.
Sprint similar manner to Speed. This mode removes any overhead time associated with
the pre-exposure ensuring minimum sample analysis time.
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d. Intelligent Uptake and Rinse
• Delays for Uptake and Wash can be defined
for the analytes added to the table.
• The Uptake starts when the signal for the
specified value for the analyte or analytes is
stable.
• If this value falls below the specified value
after the measurement has been
completed, the Wash procedure starts.
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e. Inter-Element Correction
• The Inter-Element Correction is a
corrections for direct spectral
interferences.
• Select (Enable) for the element you
wish to define the correction for.
• Select the (Enable )for the
appropriate element and enter the
formula for the correction.
• Click to save the changes
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f. Standards
• Standards are materials containing a known
concentration of an analyte.
• They provide a reference to determine unknown
concentrations or to calibrate analytical
instruments.
• The Standards section is used to enter
information about each calibration standard that
will be used to generate the calibration curve.
• Concentration ratio standards and summation to
100% are for solid.
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Commands of the Standards
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g. Quantification
The Quantification view to set the calibration and quantification strategy for each analyte.
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Quantification
• Customized Traces feature allows converting an element concentration into a
molecule concentration.
• Multi-Calibration trace will enable switching from a sensitive wavelength to a less
sensitive wavelength depending on the measured concentration.
• Internal standard is used with warning limits and failure limits of its recovery in
percent.
• Standard Range To control the calibration range. Values outside this range are
excluded from calibration.
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h. Ratios
• Allows you to define analyte ratios for the measurement.
• Displays the ratio of columns Analyte 1 and Analyte 2.
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i. Quality Control
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Quality control blank tests
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Quality control calibration tests
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Quality control paired sample tests US EPA
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Quality control spike recovery US EPA
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Quality control spike recovery US EPA
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2. Sample definition
• Sample Definition is a sub-section in
the Template view in Qtegra.
• In this section the parameters of the
measurements are defined.
• The QC settings are specified for each
sample in the Sample Definition section
of the eQuant Template in Qtegra.
• QC samples can be defined as Initial
Actions, as Continuing Actions with the
appropriate value for Interval, or in
special cases as End Actions.
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3. Automatic export
In the Automatic Export view of a Template in Qtegra, you define the export settings for your
data as *.csv or *.xml file and for reports.
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Report Export
• Upon completion of the LabBook, the data are automatically exported as defined.
• The export directory is defined under System Options in the Scheduler settings in the
Export Directory
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4. Peripherals
• Peripherals are added to the
Configuration in the Configurator tool
of Qtegra.
• The settings for peripherals can be
adjusted in the corresponding view of
the Template or LabBook in Qtegra
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Manual Sample Control
• Manual Sample Control can be added to
your Configuration in the Configurator to
enter samples without autosampler.
• In the Manual Sample Control view in
Qtegra, Uptake and Wash Time can be
defined.
• Time mainly depends on the length of the
probe capillary and the uptake rate.
• The value of the Wash Time should be
increased when going for high analyte
concentrations or tough matrices to avoid
carry-over effects.
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LABBOOKS
LabBooks contain all
information needed to run a
measurement in Qtegra
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Contents
1. LabBook Toolbar
2. Color Scheme of the Periodic
Table
3. Method Parameters LabBook
4. Summary of LabBook
5. Sample List - LabBook
6. Automatic Export - LabBook
7. Scheduling a LabBook
8. Viewing the Result of a Measurement
9. Log Messages
10. Signing
11. Query
12. Reports
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labBook Creation
• LabBooks are created from
Templates or LabBooks and are
based on the settings specified
in the respective Template or
LabBook.
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1. labBook toolbar
• Save,
• Close ,
• Run or export a LabBook,
• Unlock will only appear after the LabBook has been added to the Scheduler,
• Create a new LabBook or Template from the existing current labBook,
• Export LabBook data
• View the history of the current Template,
• Set the same order for the elements in all the tables,
• Hide the Content pane.
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2. Color Scheme of the Periodic Table
The color scheme of the periodic table of the LabBook is inherited from
the definitions in the Template.
A shortcut menu offers several color schemes for the periodic table
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3. Method Parameters LabBook
• Method Parameters are inherited from the
Template or LabBook from which the
LabBook is created in Qtegra.
• All settings of the Method Parameters can
be still be changed in the LabBook in
Qtegra.
• If you create a LabBook from a blank
Template, the Configuration currently
loaded on the Dashboard is used
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4. Summary of LabBook
A summary page is added to each LabBook in Qtegra.
This page shows the file name, and information about Properties
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5. Sample List
• The Sample List of a LabBook is
based on:-
• The number of samples selected
for analysis,
• The structure of the
o Initial Actions,
o Continuing Actions and
o End Actions items
defined in the section of the
Templates.
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6. Automatic Export
• Before measurement, you can define
Automatic Export settings for a LabBook in
Qtegra.
• Upon completion of the LabBook, the data
are automatically exported.
• LabBooks inherit the Automatic Export
settings from the Template.
• Automatic Export settings are not available
for Completed LabBooks since they have
already been exported if so defined.
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7. Scheduling a LabBook
• Click to schedule the LabBook.
• The LabBook is added to the Scheduler
• The completed LabBook is automatically
deleted from the Scheduler and added to
Completed LabBooks.
• If you wish to still change LabBook
parameters, click to unlock the
LabBook The LabBook is unlocked and
remove from the Scheduler
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8. Viewing the Result of a Measurement
• Recalculate Updates the data automatically, The button then flashes to advise you there are
some updates to be performed.
• Inter-Element Correction, Switches the mathematical interference correction on and off.
• Blank Correction Switches the Blank correction on and off.
• Use Internal Standard Switches the use of an internal standard on and off.
• Display Details Displays an enlarged graph of the calibration curve including the calculated
values for the background equivalent concentration (BEC), the instrumental detection limit
(IDL) and the most common statistical data.
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Results Intensity
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Sub-array
• During analysis, the CID detector is read in a
sub-array configuration.
• In order to reduce the read cycle time, all
analytical wavelengths are designated, as a
small array that, by default for UV is 5 pixels
tall by 12 pixels wide and for the VIS is 2
pixels high by 12 pixels wide.
• The maximum size for any Subarray is 24
pixels wide by 7 high.
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Sub-array functions
Figure shows the spectrum for a situation where an
interfering line is observed beside the element
of interest.
The analyst has many choices:
1. Select an alternate interferant free line.
2. Move or turn off the background points to
negate the interferant
3. Use an interfering element correction (IEC)
to counteract the effect of the interfering
element. This method is only applicable to
direct spectral overlaps .
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Results Concentration
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9. Log Messages
• The Log Messages view of a LabBook in
Qtegra is added to the LabBook after a
measurement has been run for this
LabBook.
• It contains all events with appropriate
time stamps which occur throughout the
manipulation of the LabBook. All
information, warning, error and service
concerned messages are logged.
• In the Completed LabBooks tab, click the
LabBook you wish to view
• Use filter in the header of the column
you wish to filter the display of.
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10. Signing
• The Signing view of a LabBook in Qtegra is
added to the LabBook after a measurement
has been run for this LabBook.
• SW provides a multi-user Signing workflow
for LabBooks.
• This workflow can be adapted to your
typical laboratory workflow. The default
Signing workflow provides the steps
Acquired By, Verified By, and Approved By.
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11. Query
• The Query view of a LabBook in
Qtegra is added to the LabBook
after a measurement has been run
for this LabBook.
• The Query and Reports view of a
completed LabBook are basically
the same as on the Results page of
a LabBook Query.
• An overview of different result
information like intensities or
determined concentration can be
displayed at a glance and can easily
be exported.
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12. Reports
• The Reports view of a completed LabBook
in Qtegra displays the reports of a
measurement in report formats previously
created.
• In the Reports view of a completed
LabBook in Qtegra, you generate result
data reports from presets.
• You can structure your report to your
needs.
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GETTING STARTE
D
Analysis with eQuant Evaluation
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Steps
1. Setting Up the Template
2. Creating LabBook for Analysis with
eQuant Evaluation
3. Run the Experiment of your Analysis
with eQuant
4. Results and Data Evaluation
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1. Setting Up the Template
1- Create a template “ select and define the
required data and
parameters on next”:
a. Analytes
b. Measure Modes
c. Acquisition Parameters
d. Intelligent Uptake and Rinse
e. Inter-Element Correction
f. Standards
g. Quantification
h. Ratios
i. Quality Control (save the changes to your Template).
2- Define settings of autosampler.
Define the settings of your autosampler
as appropriate.
3- Define Sample Definition
Define Initial Actions, Continuing Actions
and End Actions as appropriate.
(save the changes to your Template).
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2. Creating LabBook for Analysis
• Qtegra - Home Page - click Analysis.
• Enter a Name for the LabBook and select a
Location.
• Click the radio button Create a new
LabBook from an existing Template.
• Enter a number for Samples.
• Import a sample list.
• In the toolbar of your LabBook page, click
to save your LabBook.
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Getting Started notes
• The instrument is designed to be constantly powered up and the optical system
continuously purged.
• The instrument is powered via an on/off switch at the rear of the left side
• If the instrument power has been switched off, allow at least two hours after restoring
power to thermally stabilize the instrument.
• If the gas supplies have been switched off, the optical components should be purged for at
least two hours before turning on the water chiller and running samples. Doing so can
seriously damage the CID detector.
• Deionized water (or organic solvent if using an organics kit) should be aspirated for twenty
minutes to allow the instrument to fully stabilize before analysis.
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Preparing the system
1. Turn Argon Gas on at Cylinder and set for 0.6 MPa (6 BAR) pressure
on gauge near instrument
2. NOTE: for normal use gas should be left purging constantly
3. Switch on power to iCAP 7000 Series ICP-OES Spectrometer.
4. NOTE: for normal use power should be left on constantly
5. Switch on Water Chiller
6. Push Platen on to rollers of pump by way of the 4 (3) pressure screws
7. Make sure the drain tube is placed in an open neck vessel
8. Place sample tube in a blank solution
9. Switch on computer
10. Click on the “Qtegra” Icon on desktop
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Continue
11. Purge boost button at rear right of instrument On/off switch at rear left of instrument
12. Camera temperature should be - 46 °C (±2)
13. Optics temperature should be 38 °C (±1)
14. Gas supplies - Ar plasma gas 5.5 bar (80 psi)
15. N purge gas (if used) 3-5.5 bar (45-80 psi)
16. Chiller temperature set to 5 °C below the room temperature (and must be set between 15 °C
and 30 °C).
17. Torch is correctly fitted in the torch holder and the torch holder is locked into the torch box.
18. Ensure adequate provision for waste sample is made.
19. Sample tubing, particularly pump tubing, should be in good condition.
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Lighting the plasma
• Click on “Qtegra” to open the program.
• On the Dashboard Page, click on the “Get
Ready” icon to open the window.
• Define warm up time. Click “ok”.
• NOTE: To allow the plasma to stabilize leave
Plasma on with blank solution running for
about 10 minutes before carrying out an
analysis.
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LED indicators
• On the rear right hand side of instrument
there are row of LED’s which indicate the
status of the instrument.
• Once the chiller has been turned on and
has reached its set temperature LED’s 2-7
should be on and led 1 and 8 should be
flashing.
• LED 9 indicates engineer fast purge has
been selected and should be t turned off
when analyzing samples.
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3. Run the Experiment of Analysis
• Qtegra - Home Page - Analysis.
• Below Open LabBook, click The Browse for
LabBook dialog opens - Select your eQuant
LabBook.
• Click to open the LabBook.
• The LabBook opens in a new tab of Qtegra.
• In the toolbar of your LabBook, click to
schedule the LabBook for execution.
• The LabBook is added to the Scheduler.
• NOTICE If the check box Automatic has
been selected for Start Queue in the
Options settings of the Scheduler (see
“Customizing Scheduler Settings”
the measurement starts immediately.
• If the execution does not start immediately,
click in the toolbar of the Scheduler. The
execution of the LabBook is started.
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Sampling
• If using the Manual Sample
Control define Uptake and
wash times.
• If using an Autosampler define
the autosampler settings.
• On the sample list define the
samples to be analyzed.
• If using an autosampler
identify the rack and vial for
each sample.
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Running the analysis
• In the toolbar of your LabBook click “Run”
to schedule the LabBook for execution.
• The LabBook is added to the scheduler.
• If the check box Automatic has been
selected for Start Queue in the options
settings of the scheduler the measurement
is started immediately.
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4. Results and Data Evaluation
• In the Evaluation Results Concentrations view of the
LabBook in Qtegra, the results of the quantitative
analysis are summarized.
• As with the sample list, blanks are displayed in blue,
standards in yellow, QCs in red and unknowns in
white.
• The mean values, standard deviations (SD) and
relative standard deviations (RSD) as well as the
results of each main run are shown when the line is
expanded by clicking.
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Shutting Down the Instrument
• After an analysis is finished a blank sample should be aspirated for five minutes to ensure
the sample introduction components have been rinsed of sample. then deionized or
distilled water .
• For organic the final rinse should be the pure solvent. Air should be aspirated for one
minute to remove organic solvent from the sample lines and to remove organic vapors.
• The plasma should be turned off.
• Allow two minutes before switching off the water chiller and gas supplies.
• Allow five minutes after switching off the instrument, or accessories, before disconnecting
the electrical power or other supplies.
• Release the tension on the sample pump platens.