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NORAN System 7 Version 2.2
NORANSystem 7
Training Guide
C July 2004 Revised edition; added Feature Sizing System SIX 1.5
D March 2005 Revised eddition; added X-Phase, Spectral System SIX 1.6
Match, System SIX 1.7
Chapter 1
Tour of System 7 Software Interface . . . . . . . . . . . . . . . . . .1
Overview of System 7 Capabilities . . . . . . . . . . . . . . . 1
Software Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . 2
Starting System 7 . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4
Arranging the Screen. . . . . . . . . . . . . . . . . . . . . . . . . . 4
Saving Your Rearranged Screen. . . . . . . . . . . . . . . . . 5
Overview Of The Menus . . . . . . . . . . . . . . . . . . . . . . . 6
Overview Of The Toolbars. . . . . . . . . . . . . . . . . . . . . . 9
Chapter 2
Project Management . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .13
Project Explorer Window . . . . . . . . . . . . . . . . . . . . . . . 14
Creating a New Project . . . . . . . . . . . . . . . . . . . . . . . . 15
Opening a Project . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
Creating a New Template . . . . . . . . . . . . . . . . . . . . . . 16
Resetting a Project . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
Importing Files From Another Project . . . . . . . . . . . . . 16
Searching for a Project . . . . . . . . . . . . . . . . . . . . . . . . 17
Chapter 3
Spectrum Mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .19
Pre-analysis Considerations . . . . . . . . . . . . . . . . . . . . 19
Selecting Spectrum Mode . . . . . . . . . . . . . . . . . . . . . . 20
General Spectral Acquisition Procedures . . . . . . . . . . 22
Spectral Acquisition Setup. . . . . . . . . . . . . . . . . . . . . . 23
Acquisition Setup Considerations . . . . . . . . . . . . . . . . 25
Microscope Properties. . . . . . . . . . . . . . . . . . . . . . . . . 27
Detector Status . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28
Adjusting Spectral Display. . . . . . . . . . . . . . . . . . . . . . 30
Qualitative Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . 36
Using SpectraCheck After Identification . . . . . . . . . . . 45
Comparing Spectra . . . . . . . . . . . . . . . . . . . . . . . . . . . 46
TABLE OF CONTENTS i
TABLE OF CONTENTS Quantitative Analysis. . . . . . . . . . . . . . . . . . . . . . . . . . .48
Specifying Quant output . . . . . . . . . . . . . . . . . . . . . . . .53
Quantification With Standards. . . . . . . . . . . . . . . . . . . .55
Quantification For STEM/TEM Analysis . . . . . . . . . . . .62
Additional Tools in Spectrum Mode . . . . . . . . . . . . . . .67
Calibrating Fine Gain . . . . . . . . . . . . . . . . . . . . . . . . . .73
Adjusting Configurations . . . . . . . . . . . . . . . . . . . . . . . .75
Chapter 4
Electron Imaging Mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 79
Imaging Mode Interface . . . . . . . . . . . . . . . . . . . . . . . .79
Setting Imaging Acquisition Properties . . . . . . . . . . . . .80
Acquiring An Electron Image. . . . . . . . . . . . . . . . . . . . .80
Post Acquisition Processing . . . . . . . . . . . . . . . . . . . . .81
Managing Image Files . . . . . . . . . . . . . . . . . . . . . . . . . .83
Chapter 5
Point and Shoot Mode. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 85
Setting Point and Shoot Acquisition Properties. . . . . . .86
Performing a Point and Shoot Acquisition. . . . . . . . . . .86
Chapter 6
Spectral Imaging Mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 89
Setting Acquisition Properties . . . . . . . . . . . . . . . . . . . .90
Extraction Tools . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .93
Extracting data from a polygon . . . . . . . . . . . . . . . . . . .93
Extracting data from a rectangle . . . . . . . . . . . . . . . . . .94
Extracting data from a spot . . . . . . . . . . . . . . . . . . . . . .95
Extracting linescan data . . . . . . . . . . . . . . . . . . . . . . . .96
Extracting Multiple Spectra . . . . . . . . . . . . . . . . . . . . . .101
Spectral Imaging X-ray Mapping . . . . . . . . . . . . . . . . . .101
Analyzing X-ray Maps . . . . . . . . . . . . . . . . . . . . . . . . . .103
Extracting Additional Data Types . . . . . . . . . . . . . . . . .106
Compass Tool . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .111
Chapter 7
3D Visualization . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 117
Selecting Color Schemes . . . . . . . . . . . . . . . . . . . . . . .119
Chapter 8
Linescan Mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .123
Setting Linescan Acquisition Properties . . . . . . . . . . . 123
Setting Up Linescan Elements . . . . . . . . . . . . . . . . . . 124
Acquiring a Linescan . . . . . . . . . . . . . . . . . . . . . . . . . . 124
Analyzing a Linescan. . . . . . . . . . . . . . . . . . . . . . . . . . 125
Saving Linescan Files . . . . . . . . . . . . . . . . . . . . . . . . . 126
Export as *.csv Files . . . . . . . . . . . . . . . . . . . . . . . . . . 126
Opening Linescan Files . . . . . . . . . . . . . . . . . . . . . . . . 126
Chapter 9
Creating Reports . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .127
Setting Up a Printer Report . . . . . . . . . . . . . . . . . . . . . 127
Previewing and Printing Reports . . . . . . . . . . . . . . . . . 129
Copying Items to Third-party Programs. . . . . . . . . . . . 130
Chapter 10
Spectral Match . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .131
Creating a Database . . . . . . . . . . . . . . . . . . . . . . . . . . 131
Creating a Match Database. . . . . . . . . . . . . . . . . . . . . 134
Using Spectral Match . . . . . . . . . . . . . . . . . . . . . . . . . 136
Spectral Match Parameters . . . . . . . . . . . . . . . . . . . . . 137
Chapter 11
Feature Sizing and Chemical Typing . . . . . . . . . . . . . . . . . .139
Feature Sizing Setup Mode . . . . . . . . . . . . . . . . . . . . . 139
Running A Particle Analysis . . . . . . . . . . . . . . . . . . . . 152
Chemical Typing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 156
Running Chemical Typing . . . . . . . . . . . . . . . . . . . . . . 162
Advanced Feature and Chemistry Filtering . . . . . . . . . 163
Tour of System 7
Software Interface
Overview of System 7 Capabilities
NORAN System 7 is a combination of a high-performance X-ray energy-
dispersive detector and supporting electronics, and controlling software that is
installed on a dedicated computer. System 7 detectors can be connected to a
variety of electron microscopes - Scanning (SEM), Transmission (TEM) and
Scanning Transmission (STEM). Thermo Fisher Scientific offers several
models of detectors with various ultra-thin windows, resolutions, and cooling
options:
The basic System 7 (Model 102) allows you to acquire, analyze, quantify, and
create reports of X-ray spectra. With additional electronics and software
packages, System 7 (Model 202) adds electron imaging, spectral imaging, and
linescan data acquisition capabilities (with release of version 2, the only method
of collecting X-ray maps is via spectral imaging). Additional capabilities may be
added to System 7 (Model 302) through optional software packages. System 7
supports the following optional software modules:
• Compass: a statistical analysis of components.
• Direct To Phase option includes Compass, Phase Analysis (XPhase) and
Spectral Match to automatically create Phase Maps during a Spectral
Imaging acquisition and match them to known materials.
• Analysis Automation: after defining the desired parameters, this option
lets you automatically perform repetitive acquisitions on large scale analy-
ses without the need for user intervention or input (requires stage control).
Additional Options:
• Single Keyboard, Single Mouse (SKSM) - allows control of both micro-
scope and System 7 from a single mouse and single keyboard.
• Electron Microscope Column Integration - for integrating microscope
parameters with System 7 applications.
• Electron Microscope Stage Control - software for controlling microscope
stage movement from System 7applications.
• WDS Automation and Analysis - software for integrating wavelength-dis-
persive spectrometer acquisitions and analysis with System 7 EDS acquisi-
tions (requires MagnaRay spectrometer).
• Dual Detector Option - Two detectors controlled by one front end.
Software Overview
The NORAN System 7 provides complete microanalysis acquisition, analysis,
reporting, and file management. System 7 features a common, multi-pane user
interface containing a wide assortment of analytical views and controls. All
microanalyses functions are accessed from this single, multi-pane interface.
All commands are initiated through Main Menu entries with submenus. The
most common commands can also be accessed by clicking toolbar buttons.
Each analytical mode has a unique toolbar with appropriate buttons associated
with that mode. Some toolbars, such as the Acquisition Toolbar, are common to
all modes. As you switch analytical modes, the set of toolbars changes to reflect
the various functions preformed in that mode. For each mode, once set,
toolbars remain in the same location and use the same icon set. General,
program-wide operations, such as controlling acquisition and microscope
parameters and managing data layout, are accomplished through dialog boxes.
Data are saved and managed within projects. As you switch modes, the
project’s files for that mode are displayed in the File List view. Data files are in
industry standard formats - TIFF for images, EMSA for spectra. X-ray maps are
saved in TIFF format.
Navigation Coordinated
Pane Cursors
Base File
Name
Spectrum View
File List
View
Analysis
Controls
Pane
Status Bar
Spectrum Toolbar
Positioned on the right edge of the Spectrum View window.
Click on the left edge of a toolbar (control bar) and drag it to
reposition it.
Toolbars can float over the System 7 window as a separate window. To create
a floating toolbar, either drag it over a main portion of the window or double-
click the left edge (control bar) of the toolbar. To return a floating toolbar to its
original position, double-click the toolbar’s title bar. The toolbar snaps back to
its last parked position.
Restoring toolbars
It is possible to remove a toolbar from the window by floating a toolbar and then
closing it instead of returning it to a parked position. To restore toolbars after
closing, select View from the System 7 menu options, and select Restore
Toolbars from the drop down menu selections. Toolbars that were closed will
now be restored and available.
Erase All Points In Point and Shoot Mode, erases all points
on the image (before acquisition).
Help
Analysis Toolbar
Contains buttons for qualitative and quantitative analysis.
WDS Scan
Identification
Acquisition Toolbar
Contains buttons for acquisition operations, including starting, stopping,
pausing, and aborting. Also includes buttons for Acquisition Properties and
Microscope Parameters.
Acquire Averaged Microscope
Image Stop Abort
Parameters
Image Image
Intensity Ruler
Polygon Cursor
Linescan
Extract by
Image
Intensities
Spectrum Toolbar
Contains buttons for adjusting the scale and range of the Spectrum display.
Scroll Scroll
Right Down
Expand
Apply y-log
Full Scale
Spectrum
Spectrum ID Toolbar
Contains buttons for controlling searching, displaying KLM lines and peak
labels.
Polygone area
Scan area
Review shape Similar intensity area
Compass/Phase Toolbar
Contains buttons to toggle from maps to Compass components and extracting
phases.
Manually Determine Phases
from Maps
Toggle between
compass and x- Automatically Determine
Phases from Maps
ray maps
Automatically Determine
Phases from Compass
components
Project Management
Project concept
A project is essentially a folder created by the user for storing and organizing
Noran System 7 data. In addition, a project includes various parameters -
element lists, identification configuration, quantification data and acquisition
properties. The initial parameters are stored in a “template” which is selected
when a project is created. The template parameters are updated when various
parameters are changed during use. Acquired data are stored, along with their
acquisition properties, within a project using a base file name(s). Each project
can consist of several subprojects.
When you close a project, System 7 will automatically ask if you want to save
the acquired or altered file(s) within the current project. If you choose to save
the data within the project, the file(s) is moved from the project's temporary
folder to the main project folder. The temporary folder is then removed along
with any non-selected data. If NS7 is closed, or electrical power is lost, without
first closing a project, the temporary folder and all contained data are main-
tained. If you are working with data stored in the temporary folder (not yet
saved to a project) and experience a power failure, the data will be in the
temporary folder when you restart System 7. Thus, all acquired data are never
lost due to accidentally closing System 7 or by power failures.
Properties Tab
3.
Opening a Project
Follow the steps below to open an existing project:
1. Click the Project Explorer button (or from the File menu, select
Project Explorer).
If any other projects are currently open, System 7 prompts you to save or
discard the data.
Resetting a Project
Resetting a project restores the template settings for that project.
To reset a project, open the Edit menu and select Reset Project.
Any changes to the settings are returned to the settings for the original template
file used for the project.
Note: If the template settings have changed during the time between when the project
was created and the time the project was reset, the project will be reset to the
original template’s current settings.
Spectrum Mode
This chapter discusses the System 7 Spectrum mode and its associated
components. An in-depth look at the tools for setup, acquisition, qualitative
analysis, quantitative analysis, and energy calibration is included. These tools
are common for any analysis mode that includes a spectrum, such as Point-
and-Shoot and Spectral Imaging. Before discussing the Spectrum mode, there
are some general concepts to consider before performing any microanalysis.
Pre-analysis Considerations
Sample preparation, microscope operating conditions, and detector geometry
all have an effect on the accuracy of EDS analyses. This section provides
general guidelines to consider before performing an analysis.
Sample preparation
The first step with any analysis is sample preparation. It is highly recommended
that samples are flat, well polished, and electrically conductive. If the sample is
not flat and polished, be aware that some topography may affect the line of
sight to the detector. A conductive coating should be applied to samples that
are not electrically conductive, or use variable pressure if you have this type of
SEM. When you apply a conductive coating you are putting an element into the
spectrum, such as carbon or gold, that may not be present in the sample.
Elements of the coating material must be noted and accounted for if a quanti-
tative analysis is to be performed.The thinnest useful coating of carbon is best
for the majority of samples. Be aware that coatings with high atomic number
materials will absorb x-rays of low atomic number elements within the sample.
Spectrum Display/
View Pane
There are 3 main Window Panes associated with Spectrum Mode: Spectrum
Display Pane, Analysis Control Pane and the Information Pane.
Tab Functions
Element Setup Displays identification results, allows selecting or
excluding elements for analysis, selecting elements
to view KLM markers.
Quant Results Displays results of quantification analysis .
Parameters displayed are selected from the main
menu Edit > Properties > Quant Results tab.
Analysis Setup Setting parameters for identification sensitivity, type
of matrix correction and quant fit methods.
Processing Allows toggle on/off auto ID, auto quant, auto
extract for Spectral Imaging and selection of
quantification for x-ray maps and linescans.
Compare Selection of spectra, synthesized spectrum, and
Information background for comparitive overlay views of a base
spectrum.
Analysis Automation Optional software package. Setup for multipoint
automatic analyses
Information pane
The Information Pane has 6 tabs which present information about the displayed
spectrum.
Tab Functions
Attributes Displays acquisition information about the acquired
spectrum. Details button provides additional
information. These attributes are stored with the
spectrum.
Notes Allows adding additional notes and information
about the displayed spectrum. These are stored
with the spectrum.
Detector Status Displays information about the detector.
Standards Available when using quant with standards.
Displays information about the standards used in
the project.
Match Results Displays results from Spectral Match.
Region Tool Displays mathematical results from regions of
interest in a spectrum.
Termination Criteria
Live Time Limit The duration of the acquisition in live time seconds. A
general rule for spectral acquisition is 100 seconds of
live time collection at 25-30% dead time using the 50
usec time constant.
Line Select the x-ray line for the element of interest to define
the region of interest.
User Defined Allows the user to redefine the low and high eV values
for the region of interest. Max Counts terminates the
acquisition. If all termination limits are set, the first
reached limit will terminate the acquisition.
Energy Range
Low energy X-ray counts below this energy are ignored during an
cutoff EDS acquisition. This cutoff eliminates the “noise” peak
in the low energy region. Auto adjusts the energy value
according to the Pulse Processor Time Constant. Each
time constant has a unique noise level.
Max keV X-rays of energy up to this limit are included in the EDS
acquisition. Typically, 20 keV will include an x-ray line
from all elements using a scanning electron
microscope. For TEM, 40 keV is appropriate. Auto
changes the energy limit according to the microscope
kV.
Pulse Processor
Time Constant Select a time constant. Rate 8 has the worst resolution;
Rate 2 or 3 has the best resolution. Rate 3 or 4 is a
general, all-purpose time constant. Auto adjusts the
time constant to keep the dead time between 30% and
50%. Depends on the beam current and accelerating
voltage.
If values, other than 0 or blank, are entered in the termination section, the first
reached criterion will terminate the acquisition (zero equates to infinite).
The Low Energy cutoff clips the energy display range from 0 eV to the value
entered in the edit box (clips off the noise peak). The Auto selection will adjust
the cutoff value depending on the estimated noise at a given pulse processor
time constant. Generally a value of 100 to 120 will eliminate the noise peak at
the low energy range for most time constants.
The Max keV energy range selection determines the number of channels allo-
cated in memory (each channel represents 10 eV). For example, if a maximum
keV range of 10 keV is selected, 1024 channels of memory will be allocated. At
this range any peak greater than 10.240 keV will not be saved nor displayed.
In selecting the maximum range, the pull down menu gives the following
choices: Auto, 5, 10, 20, 40, and 80 keV. The Auto selection will automatically
adjust the maximum range to the accelerating voltage of the microscope. If the
accelerating voltage is not entered correctly, the range may be incorrect. Fixing
the maximum range to 20 keV for an SEM will provide consistent spectra for
comparison.
Pulse processor
The pulse processor time constant is the time allowed for the pulse processor to
estimate the energy of an x-ray. The longer the time, the better the estimate of
the energy. The better the estimate, the higher the resolution of the peak.
However, the longer the time constant, the higher the dead time for a given
count rate. For high resolution spectra (long time constant), this translates into a
lower count rate and a longer time to acquire a statistically valid spectrum.
For high resolution (extreme) detectors, there are 10 fixed time constants plus
the Auto selection. Non-extreme detectors have 9 fixed time contants plus the
Auto choice. All fixed rates have estimated through-puts (counts per second).
Care should be taken when using the Auto selection. System 7 will adjust the
time constant to achieve between 30% and 50% dead time. At high beam
currents, the time constant will be shorter and spectral resolution will degrade.
Microscope Properties
For any analysis, the accelerating voltage of the microscope must be known by
System 7. Various parameters, including the accelerating voltage, are entered
in the Microscope Properties window. To open the Microscope Properties and
Status Bar Selection dialog box, click on the Microscope Properties
button, or from the main menu Edit > Microscope Properties. Enter the accel-
erating voltage in the edit box. This dialog box also allows for displaying various
parameters on the status bar. If optional Column Automation software is
purchased, these parameters are updated automatically.
Detector Status
In Spectrum mode, the bottom right pane (Information Pane) provides infor-
mation about the acquired spectrum, allows additional information about the
acquired spectrum to be noted, status of the detector, and, if using analysis with
standards, provides information about the standards in use. The Detector
Status tab provides information about the condition of the detector and events
occurring with an acquisition.
Group Description
PHA
Zero FWHM The full width half max measure of the zero peak
(the noise peak). Zero FWHM indicates the level
of random noise in the system. Small FWHM
indicates a “quiet” detector system. This gives
some indication of the system resolution.
Current Times
Remaining Time Shows the remaining Live Time for the current
acquisition. With no acquisition, displays the
duration of acquisition set in Acquisition
Properties: Live Time Limit.
Spectrum
Properties
Spectrum Tab
Click on colored
boxes to change
colors
Spectrum Toolbar Full View Expand Scroll Right Scroll Log y-scale
Down
Use these buttons to adjust the
spectrum range
Most of these functions conincide with
mouse and keypad functions
Scroll Left Compress Scroll Up Full Verticle Scale
Place the energy cursor near the energy range of interest and click the Expand
Spectrum button on the Analysis Toolbar. The spectrum will expand and
keep the cursor near the center of view.
Zooming in on a peak
To zoom in on a portion of the spectrum, hold down the Ctrl or Shift key and
drag the mouse pointer across the peak.
Saving a spectrum
Acquired spectra in Spectrum Mode are stored automatically in the temporary
folder (associated with the open project) with the .emsa file extension. The user
will be prompted when a project is closed, or a new project is opened, if the new
files should be saved.
Auto Quant
When Auto Quant is active, System 7 calculates the quant information and
displays it in the Quant Results tab. If Auto Quant is active, Auto ID must be
active.
Processing tab
The bottom left corner of the Spectral Display Pane shows the symbol of current
element that has its KLM markers displayed.
Labeling a peak
Labeling all peaks for one element
Right-click on the element in the Element Setup
periodic table and select Identified.
SpectraCheck toggle
active/inactive
Comparing Spectra
You can compare two or more spectra in the Spectrum Mode.
1. Open a project and go to Spectrum Mode.
2. Load a spectrum. This is the base spectrum.
3. Click the Compare Information tab in the bottom left pane.
4. In the Spectrum section, check one or more spectra to compare against
the base spectrum. With Spectra Check active you can also select a
synthetic, background, or residual spectrum:
• Synthetic – Based on the elements identified in the periodic table, System 7
calculates how the spectrum should appear and generates this synthetic
spectrum.
• Background – The synthetic background spectrum.
• Residual – The peaks of the elements defined in the periodic table used for
generating the synthetic spectrum are removed from the spectrum to create
a residual spectrum. This spectrum shows what peaks were not accounted
for in the original spectrum.
Note: A theoretical model of the background shape and spectrum can be created if
the approximate mass of the sample, the energy of the excitation electrons, the
geometry of the system, and detector characteristics are known. Generation
Overvoltage
On the Analysis Setup tab, select the Overvoltage amount. Typically, the accel-
erating voltage should be 1.5 to 2 time greater than the highest x-ray energy
line. This value is used by System 7 to select a dominent x-ray line.
6. When System 7 completes the analysis, click the Quant Results tab in the
Analysis controls pane to view the results.
The lower the Chi-squared value, the better the fit. A perfect fit is 0; as a
general rule, a Chi-squared value under 10 is good.
There are a number of parameters that are calculated during the Quantification
routine. To select which parameters you want displayed with the quant results
use the Quant Results tab on the Properties window.
1. From the Main Menu: Edit: select Properties.
2. Select the Quant Results tab on the properties window.
3. Select the parameters you want displayed. These parameters are
displayed in the Quant Results tab in the Analysis Controls pane.
4. An s by the element indicates stoichiometry
5. Click OK to close window.
• Normalization, Total Weight%: The default is 100%. If you know the com-
position of the sample, you can type in a Total Wt% value. Generally, for
standardless analysis, normalize to 100% is the standard value.
• Output X-ray Lines: All will show the x-ray lines that are displayed in the
spectrum. For example, All will list the Ka and La for Cu in the quant results
tab. However, only the dominent line will be used for quant. In this example
the Cu Ka will have a quant value and the La will have no value. Matrix
Only will only display the x-ray line used for quantification. In the example
Creating standards
Before creating your standards, use the following guidelines to make the
standard as accurate as possible.
• Use a standard that is flat and well polished. If the standard is non-
conductive, coat with a thin (<5 nm) layer of Carbon - just enough to
keep from charging (or use variable pressure microscope).
• The standard should be well characterized with known weight percents.
A “traceable” (NIST) standard is preferable.
• Count for sufficient length of time to obtain minimually 10,000 integrated
counts. Ten thousand counts results in a 1 Sigma error of 1%.
• Use the longest fixed pulse processor time constant rather than Auto.
Adjust the beam current to get a dead time of about 25 - 30%.
• Collect the unknown sample under the same conditions as you
collected the standard. That is the same working distance (should be at
optimal working distance), detector fully inserted, and same beam
current. The exception is that the beam current can vary because
System 7 adjusts for beam intensity differences (the standards are
calculated in counts/second/nA of current).
unchecked. This will close the New Standard window and put the new
standard into the Add Standards dialog window.
17.Add more standards to the Standards Database list if desired. You can
create a database with many standards, or just one standard.
18.For convenience, add all element standards you expect to find in the
unknown.
If your standard has more than one element (multi element standard) check the
Multi Element Standard box.
Select the Concentration Data Type from the pulldown menu. This will display a
multi element data section. Enter the known values for the data type. You will
need to do repeat these steps for each element in the standard, entering one at
a time.
To use a standard
To activate a standard, or standards, use the following procedures:
Defining K-factors
There are 2 ways to enter/define K-factors: manually calculate and enter the
values, or automatically calculate and enter the values through System 7
software.
Manual method
To manually calculate K-factors you need to acquire a spectrum of a sample
with known concentrations (i.e. a NIST or similarly well characterized standard)
using the same acquisition parameters as the unknown - beam current, acceler-
ating voltage, count rate, etc. After spectral acquisition, a quant must be run to
obtain the net intensities for the reference element and the desired element.
Typically, Si is used as the reference element. Not all standards will have all the
elements, including the reference, of interest. You can calculate the K-factor for
an element against the reference using an intermediate K-factor using a
different reference element.
Adjust energy
range
17.After adding all elements, select all the elements just added in the
Standards Database (Add Standards window) and add to the Standards in
Use (select and click on Add Selected button).
18.Click OK to add to the Standards in Use on the Standards tab.
The elements with calculated K-factors are now in the Standards in Use on the
Standards tab (Information Pane).
Batch processing
You can quantify a number of spectra and save the results as a .csv (comma
separated values) file which can be opened in a spread sheet application, such
as Microsoft Excel, for further mathematical analysis.
To batch process spectra, Sum Peak removal, Escape Peak removal, Auto ID
and Auto quant must be ON. From the Main Menu Batch Processing, select
Quant Analysis from the submenu. A Select Files... window will be displayed.
While holding the Ctrl or Shift key (same function as in Windows operating
system), left click on the spectral files you want processed.
After selecting files to process, click on Open button to begin processing. A File
Save.... window will open. Enter a file name for the .csv file.
The Fine Gain calibration makes final corrections to peak position. This
procedure should be used if peak positions are not correct.
1. Select the Service Mode tab and click on the EDS Calibration Icon.
2. Click the Auto tab in lower left corner of the EDS Calibration mode to
display the Fine Gain calibration settings.
3. Put a clean Manganese (you can use any element, but Mn is the industry
standard) sample in the microscope.
• Minimum accelerating voltage of 15KV.
4. In the Setup section of the window, select Mn as the Atomic Symbol, K as
the Line, and 30 for Maximum Iterations using the pull down selections.
5. Select a Time Constant from the drop down selections.
• The program will move the peak selected to the energy value of
Manganese that was selected in step 4.
• The new Fine Gain setting and the Calibration Date will be updated in
the status section in the right hand section of the Auto tab.
9. Repeat steps 4 - 8 to calibrate the Fine Gain for all available Time
Constants.
NS7 Instrument
Configuration mode.
7. In the EDS Detector section, enter the appropriate values to describe the
installed detector.
• Detector name: Type a name to be used for the detector.
• Extreme Detector: Check the box if the detector is 129 eV resolution.
This will add the Extreme Time Constant setting (100 microseconds).
• Azimuth Angle: Horizontal angle, in degrees, between the EDS detector
and the direction of stage tilt. Refer to the detector drawing for the angle
information. These values are used for matrix correction if the stage is
tilted during EDS acquisition.
• Incline Angle: Angle, in degrees, at which the EDS detector is mounted
on the microscope. Refer to the detector drawing for the angle
information. Typically, the detector is a “high angle takeoff” and is limited
by the microscope construction.
• Initial slide position: Position, in mm, of the EDS detector slide when the
detector is fully inserted. Refer to the detector drawing for desired
position. Input actual value.
• Intersection distance: Vertical distance, in mm, from the microscope pole
piece to the EDS detector crystal center line. Refer to the detector
drawing for distance information. This is the optimal working distance
with the detector fully inserted.
• Crystal Tilt: Angle, in degrees, at which the EDS detector’s crystal is
mounted. Refer to detector drawing for angle information.
• Crystal Area: The area, in square mm, of the EDS detector’s crystal.
Refer to detector specification sheet for area information.
• Crystal Material and Thickness: Select the crystal type from the drop
down list and verify the proper thickness, in mm, is specified. Refer to
detector specification sheet and default values provided below.
8. Click the Apply button in the lower right hand corner to apply the changes.
Saving configurations
1. From the Instrument Configuration mode, click the Save button (or
from the File menu, select Save)
• A Save As window will appear.
Notepad area
Analysis Automation
setup tab (optional
software module)
Field Description
Overlay transparancy
factor for Spectral
Imaging mode.
Brightness and
Contrast slider bars
Micron marker in manual brightness
location check and contrast mode.
box
Auto brightness
and contrast
Hot pixel
supression mode
Ruler
Click on the Ruler button in the Extraction tool bar to display the ruler
line in the image. Left clicking and draging on either end of the ruler line will
lengthen or shorten the line. Left click and draging the middle of the line will
move the entire line. The length of the line is displayed with the line.
Ruler line
Batch processing
In imaging mode, a series of images can be stitched together to create one
larger image (Montage). However, the images must be collected through
the optional software mode Analysis Automation.
Point and Shoot has two acquisition modes: Immediate and Batch
(multiple). In the immediate mode, spectral acquisition begins immediately
after defining the point or area. The batch mode allows for a series of points
or areas to be defined then begin an automated sequence of spectral acqui-
sitions. Also you can use the P&S Select tab in the analysis controls pane to
specify which points and areas to display on the image. You can also use
the tab to select for deletion a point or area that has not yet been acquired.
Spectrum
View
Image View
Immediate Acquisition
Button Depressed
Batch Acquisition
Button NOT Depressed
Review Location
3. Click on the image at the location where you want to begin the
acquisition. In spot mode, acquisition starts when you click the point.
For area modes, acquisition begins when you complete selecting the
area.
4. Wait for acquisition to complete, or you can move the spot/area to a
new location before the acquisition completes. The new location will
have the same number as the original.
5. To add another point, click a new location.
Note: System 7 begins a new acquisition at each new cursor position under
the base name appended with point number.
Batch acquisitions
1. Click the Batch Acquisition button on the Point and Shoot
Toolbar. Leave the button NOT depressed.
Batch processing
After acquiring spectra from a number of points or areas, you can quantify
all spectra in the P&S file at one time rather than manually quantifying one
at a time. When exporting to a report, the data are organized in such a way
that they can be further analyzed, such as calculating average Wt%.
In level 300 (model 302) and higher you can also acquire phase maps
during an acquisition (Direct to Phase option).
Avg. Counts per Pixel The acquisition will terminate when the total x-ray
Limit counts in a pixel reaches this value
Element Map Vertical The acquisition will terminate when the vertical
full scale of the accumulated spectrum reaches
Full Scale
this value
Once the Spectral Imaging data set is acquired, you can extract spectral
data from areas of the electron image for spectral analysis.
The Extraction Toolbar contains buttons to specify an area of the electron
image for analysis. To preform and auto extraction, click the Auto Extract
ON in the Processing tab.
“Magic Wand”
Polygon Extraction by Image
Intensities
Linescan Image
Intensity Ruler
Cursor
When the area is drawn and the left mouse button is released the cumu-
lative spectrum from all contained pixels is created. The spectrum
appearance and the identification depend on the Spectral Processing
settings. X-ray maps are extracted from the entire image.
• The rectangle can be moved to another location. Move the mouse
pointer into the rectange and it will change to a 4-way arrow. Hold
the left mouse button and drag the rectangle.
• Extracting from entire image. The rectangle has a small square near
the upper right corner. Clicking on the square will expand the
rectangle to fill the entire image. Clicking again will reduce the
rectange to its original size.
Fat Spot
When you place the spot, the cumulative spectrum is extracted. The
appearance of the spectrum and the identification depend on the Spectral
Processing settings.
Analyzing linescans
The electron image and the linescan data use the image intensity cursor. As
you move one cursor, the other cursor moves as well. Click the image
intensity cursor button in the Extraction Toolbar to activate the cursor
Coordinated cursors
The spectrum from the point at the cursor location is displayed in the
spectrum pane (lower right pant). You can also change the results param-
eters to Wt%, Atom%, K ratio or Net Counts. Click on the Processing tab in
the Control pane and from the pull down menu in the Automatic group
select the analysis parameter you want. Redraw the line to extract and
process the data.
To overlay a data set for an element on the line, click on the desired elment
in the linescan data display.
To change the element data overlay, right click on the image and select the
Linescan Overlay tab in the General Properties window. You can choose to
have the overlay on the linescan or at the bottom of the image. For multiple
elements, you can choose to have them stacked or overlayed and also
scaled separately.
2. Selecting the magic wand tool will open the Image Intensity Selection
window.
3. In the Cursor Diameter edit box, enter the size of the cursor as a
percentage of the image, or size in microns. If in microns, check the
Diameter in Microns check box. The cursor diameter is the size or
number of pixels around the mouse pointer that will be evaluated.
4. On the Similarity slide bar, adjust the percent similarity in intensity to
include in the selected area. If the area selected appears spotty or
does not include all the area of interest, decrease the percent
similarity. A lower percent will include more pixels.
5. Click the Extract Maps button in the Extraction Toolbar. The new
map set is created in the upper right pane.
Automatic extraction
Spectral identification and extracting x-ray maps may be performed auto-
matically.
1. Click on the Processing tab in the Analysis Control pane.
2. In the Results group, toggle AutoID to active.
3. In the Automatic group, toggle Auto Extract to active.
• When preforming an extraction, spectra will be automatically
extracted and an auto ID processed. After auto ID, x-ray maps will
be automatically extracted for the elements in the auto ID list.
After performing the initial extraction, you can add or remove elements from
the map display.
To add or remove elements from the maps, mark the elements in the
periodic table as Identified or Inactive. Click the Extract Maps button.
The new maps appear in the Maps pane.
Click the image intensity cursor button in the Extraction Toolbar to turn
it on or off.
The default color for the image and x-ray maps cursors is red. To change
the color, right-click on the image and select a different cursor color in the
General Properties Image View tab.
Note: Both the image intensity cursor and the Spectral Imaging extraction cursor
can be toggled on and off. If both the extraction cursor and the image
intensity cursor are visible, the mouse controls the image intensity cursor.
To use the extraction cursor, turn the image intensity cursor off by clicking
on its button in the Extraction Toolbar.
Map Properties
Move the mouse to the desired map
and right click to bring up the Map
Properties dialog box
Use the Map Color drop down arrow
selections to change the color of the
map.
Brightness and contrast can also be
adjusted in the manual mode
Map Properties
Select Contour
Map
Contour
Outline + Fill
gray color
Additional Tools
Extract/Maximal Button
When extracting spectra from an SI file, you can select to extract the
Maximal peak counts using any extraction tool. The button at the top of the
reference image toggles between Extract which presents total x-ray counts
from the entire extraction area or Maximal which remembers the maximum
counts for each channel in the area. The Maximal option aids in finding
small concentrations of an element, or small, localized areas of an element
which would otherwise be lost in the total background.
Single Pixel
Using compass
1. Acquire a Spectral Imaging data set, or open an existing Spectral
Imaging file.
2. Click on the Compass button in the Compass tool bar (the button will
be depressed and the Maps button will change to Components)
When Compass has processed the data, the component maps are
displayed in the top right pane of the Spectral Imaging interface window.
Each component map represents one unique component in the sample.
The first component consists of those elements with the smallest co-
variance. The second map consists of those elements with the next largest
co-variance, and so forth.
The spectrum displayed in the spectrum pane (lower right pane) is, by
default, the spectrum of the first component (the map labeled C1). To
display the spectrum from other components, click on the map image.
To change the color of the map, right click on the map and change the color
in the Map Properties, Map Color tab. You can configure the Component
maps the same way as x-ray maps.
Use the Low Energy Cuttoff (eV) to eliminate the noise peak if present in the
data set.
Set the number of Components you want displayed. Generally use the Auto
(0) choice when first analyzing an unknown data set. You can then lower
the number. This combines components with close co-variance.
3D Visualization
3-D Visualization mode lets you view a three-dimensional representation of
various types of map data. First use the appropriate mode to display the
desired type of data, and then switch to 3-D Visualization mode to view and
manipulate a 3-D image. For example, if you have displayed x-ray map data
using Spectral Imaging mode, you can view a 3-D image of the distribution
of x-ray count values for an element over the measured sample surface.
To change the appearance of the 3-D view use the general Properties
window - Main Menu Edit> Properties. The first tab is the 3-D properties.
Select the properties you want to change, and click Apply then OK to see
the changes.
Color Description
Scheme
The color bar below the Color Scheme box shows the colors used in the 3-
D image. The scale below the color bar indicates the values of the colors.
The vertical bars on the color bar indicate the limits of the value range
currently used for the colors in the 3-D image. You can change this range
by horizontally dragging the vertical bars. This in turn changes the distri-
bution of the colors.
If one or both of the vertical bars have been moved away from the ends of
the color bar, you can drag the portion between the vertical bars to the left
or right. To specify a different color scheme for the data, select the desired
option in the Color Scheme box.
ved away from the ends of the color bar, you can drag the portion between
the vertical bars to the left or right. To specify a different color scheme for
the data, select the desired option in the Color Scheme box.
You can rotate the 3-D image in any direction to see the data from different
angles. Simply drag the image in the direction you want to rotate it; the
image rotates as you move the mouse. Release the mouse button when
you have displayed the desired view of the data. If you release the mouse
button while the mouse is moving (and the image is still rotating), the image
will continue to rotate. This can help you study the shape of the data from all
sides.
To move the image to a new location within the pane, hold down the Shift
key and drag the image.
Cursor Description
Style
Linescan Mode
System 7’s Linescan Mode allows you to acquire an electron image and
linescan data. After the acquisition, analyze the linescan using the image
intensity cursor. You can save and load standard linescans in this mode
(with qualifications, as described in this section).
Note: Prior to a linescan acquisition, you must have knowledge of the sample’s
elements. This can be learned from a Spectral Imaging data set or Spectral
acquisition. If you already know the elements of interest you can mark them
on the periodic table.
Field Description
Number of Scans The number of times the electron beam scans the
line.
Acquiring a Linescan
Once the elements and acquisition properties have been defined:
1. Switch to Linescan Mode.
2. If you have not already acquired an image, click the Acquire Image
button .
3. Once the image is acquired, click on the image and draw the line
across the image.
4. Click on the Go button. The linescan acquisition will start and
data will appear in the linescan view.
Analyzing a Linescan
Once the linescan is acquired, the data appears in the top right view.
Linescan Mode
To analyze the linescan, click and drag either the image intensity cursor or
the Linescan cursor. The cursors are coordinated to move to the same
point.
Linescan element data can be overlayed on the linescan in the image the
same as with Spectral Imaging Linescan extraction.
Creating Reports
System 7 provides two methods for creating reports:
• Printer report generation
• Copy and paste reporting
Printer report generation is automatically set up in System 7. You can
customize the items you want to appear in the report and preview the report
before printing.
Copy and paste reporting uses a third party word processing, spread-
sheet, or page layout program to create the report. System 7 includes a
copy function that transfers the material in the current view into the
Windows clipboard for use by another program.
Print Preview button on the Main Toolbar (or from the File menu, select
Print Preview).
If the report is acceptable, send it to the printer from the preview by clicking
Print.
To print the report from the main System 7 screen, click the Print button
on the Main Toolbar (or from the File menu, select Print).
3. Click the Copy button on the Main Toolbar. This places the
current view into the Windows Clipboard.
4. Switch to the third-party program (using Windows taskbar, Alt-tab, or
other method to switch programs).
5. In the third-party program, use Edit > Paste or Ctrl-V to paste the
copied material.
Edit the third-party document as needed.
6. To copy additional items, switch back to System 7 and select the next
view. Repeat the process above.
Spectral Match
With Spectral Match optional software an unknown sample spectrum can be
searched against a database of previously identified spectra for quick identifi-
cation.
Before using spectral match, a database must first be created. From a large
spectral database, smaller databases may be created.
Creating a Database
Use Database Manager to manage spectral databases, including creating
them, adding spectra to them and organizing them into groups.
On the Analysis Setup tab click on the database browse button to open the
database manager.
To begin you must first add, make available, spectral files for a match database.
(the match database is by default located in the C:\NSS Libraries\Matchdata-
bases folder, but you can put them anywhere). You can make available files
from a spectrum that is currently displayed (From Spectrum), or you can import
a spectrum from any project, or you can manually add a file, or you can add
from a CSV file of an analyzed spectrum.
From Spectrum: Open a spectral file in Spectrum mode. Click on From
Spectrum button. The infromation from the displayed spectrum will be added to
the available match files pull down box in the Database Manager.
Import: Clicking on the import button will bring up an Open window which you
can browse other projects or folders to import a spectrum and add to the
Available Match Files folder.
Manual: You can manually enter elements and composition to create a Match
file. Click on the Manual button to open a form for entering data. Enter the
elements and data type in the boxes. Then click Define for Match, then Close.
The file will be in the Available Match Files.
From CSV: You can also enter spectral data into the Available Files from CSV
files. CSV files can be created directly through Batch Processing in Spectrum
mode. These files can then be used to create Available Files for Match. Click on
the From CSV button to open the Create Simulated Spectrum from CSV files
window. Select the desired file. Click on the Define for Match button to enter
into the Available Files pulldown box.
1. Click on the Match Database browse button on the Analysis Setup tab.
2. In the Database Manager window, move the mouse to the Current
Database edit box and left click.
3. Type in a name for the database. The Create Database button will now be
active.
5. In the Available Match Files pulldown box, highlight the files you want to
add to the current database. Hold the Shift Key or CTRL Key to select
more than one file.
6. Click on the Add To Database button to move the selected files into the
Currently in Database box.
7. Click Close button to save the database. This database is now the active
database for Spectral Match.
Changing a Database
You can create a number of databases for convenient use. To activate a
database, click on the Match Database browse button in the Analysis Setup
tab.
Manual match
1. Acquire or open a Spectrum
2. Click on the Spectral Match button in the Analysis
Toolbar.
3. Click on the Match Results tab in the Information pane to view results.
In the Match Results tab, the matched spectra are listed in order of the least
Chi-squared value to the highest Chi-squared value. The lowest Chi-squared is
the best fit. A Chi-squared value of 0.0 is a perfect match.
Use Match Cuttoffs (eV) to set the low and high eV range. The defaults are 0
and 10000 (10 keV). These values work for most unknowns.
The number of match spectra is set in the Max. Number of Match Results edit
box. The default is 5 which is usually sufficient. However you can display more if
desired.
Set the maximum Chi-squared value in the Chi-square Cutoff edit box. The
default is 5 which works well for most unknows. However, you may need to
increase this number to include more matches. Generally, a Chi-squared value
of less than 10 may be a reasonable match. The number of background
channels greatly influences the Chi-squared values.
There are two tools to threshold an image in the System 7 software. (1) the
Video Line Profile intensity cursors, or (2) the Selected Area Histogram
intensity cursors. Both work in conjunction; thus, you can move back and
forth between the two panes to adjust the intensity range to segment just
those features you desire.
High and
low intensity cursors
Histogram across
line profile
To add an other
phase, click on the +
button in processing
group
Phase 1
Phase 1 and 2
Advanced Processing
At times, you may want to modify how features of interest are defined and
processed. There are two additional groups of parameters available which
modify how features are processed. These are Advanced Image
Processing and Advanced Particle Processing. These parameters are
referred to as sieves or filters. The sieves in Feature Sizing are cumulative,
meaning that particles must pass all filter criteria before being stored to the
data file.
Image Processing group
Thresholding intensity
range
Advanced Image
Processing button
Advanced Particle
Processing button
Processing Pane
Guard Region
When features of interest lie on the edge of the image and are not fully
visible, some bias in the results occur because the overall size and shape of
these features cannot be determined. You can select a guard region to
avoid biasing data with partial features.
Advanced Image Processing Group with Guard Region and Basic Filters
None
No guard region is used. All particles are included.
Center of Mass
Guard Region
Excluded particle
Included particles
Guard region
Excluded Particle
After selecting a guard region, define its width. You can either type in the
width in the Guard Region edit box, or select a size from the pull down
menu. You can also use the mouse and drag the region delimiting (blue)
line. The % width of the image (frame) is automatically calculated from the
image size.
Fill holes
Runs a dilation filter to fill particles which have holes (voids) inside the
perimeter.
Particle Processing
In the particle processing group, there is only one check box and the
Advanced button. The check box turns Chemical Typing on or off. The
Advanced button brings up the Advanced Particle Processing dialog box
which allows control of what you want to measure in the sample, define
parameters used during chemical typing, set particle sieves, manage
spectra and image acquisitions for Extended Acquisitions, and set termi-
nation criteria for automated analysis.
Morphology Tab
Morphology refers to the size, shape and measurements of the particles of
interest. Morphology parameters are divided into two groupings, Particle
and Frame, and Analysis of Subparticles and Saving the locations and
microscope parameters for particles.
Analyze subparticles
Chords are the intersections of test line lengths with groups of pixels that
are turned on in a binarized image (particles). Feature Sizing scans the
image line by line, locates points where horizontal test lines intersect with
particles and then measures the length of each line segment or chord.
Feature sizing automatically determines chord length distributions for
particles.
A particle is composed of a number of smaller subparticles, as determined
by the intersections of the test lines (chords) with the particle. Checking the
Analyze Subparticles box will command System 7 software to run an
analysis on the subparticles of each particle that passes sieve and guard
region operations.
Return to particle
The Return to Particle setting automatically selects Location and Micro-
scope parameters to ensure that System 7 acquires the stage and beam
infomation it needs to visit a particle after analysis is complete. These
parameters provide the information for the “Move To” feature to set the
selected particle in the center of the field of view on the microscope.
Diagrammatic representation of
some parameters in Particle Sizing
The lower right pane has three tabs: 1) Particles; 2) Frames, and; 3)
Particle Count Summary.
Histogram of
Particle
Analysis
Particle
Analysis
Results
The Particle Results pane four controls at the botton of the pane: 1) Close
button which closes the *.siz file; 2) Move To button which moves the Stage
to the coordinates of the selected particle (highlight a particle then click
Move To button); 3) Apply Filter check box which filters the displayed data
(not the particle analysis filters), and; 4) Setup Filters button which sorts
and filters the displayed data.
To change the displayed results, check the Apply Filters check box. The
filter parameters are setup using the Setup Filters button.
Setup Filters
Select the parameter to
use as the sieve from
the pull down menu.
Chemical Typing
Chemical typing is a powerful EDS tool used in conjunction with Feature
Sizing. Features on a sample can be recognized and then chemically
analyzed and categorized into defined types.
The chemistry of sample features can be first “learned” and from the
learned chemistry, the features can be chemically categorized. In addition,
images of the specific features can be acquired and saved and spectra from
a specified chemistry can be acquired and saved.
To create a chemical library, select the Chem Lib icon in the Feature Sizing
analysis group in the Navigation Pane. The Chem Lib mode provides for
various chemistry library functions.
1. In the Chem Lib mode, select (highlight) the Chem Lib folder.
2. Right click on the Chem Lib folder and select New Library from the
submenu to create a library. This folder will have a green folder
symbol and be named “New Library.”
Advanced
Particle
Processing
button
The following figures display the results of two runs on an sample. The first
figure shows an unseccussful run in which the spectral acquisition time and/
or counts were not sufficient to chemically type the particle. The second
figure shows a successful run.
Sieves
In advanced filtering, particles must pass ALL criteria to be included in
further processing. Virtually any or all morphological, chemistry types or
element concentrations can be used to restrict particle processing.
In this setup only particles that are between 0.5 and 50 square microns
AND (ALL criteria must pass) have a chemical type of Learn 2 will be
processed. All others will be ignored.
In this setup images of particles that are between 1 and 30 square microns
in size OR (ANY of the critera must pass) have a copper content of 50 wt%
or more OR have a gold content of 50 wt% or more will be acquired and
saved.