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Operating procedure of EDS system on JEOL 2010F (See separate procedure for operation in STEM mode) Nicholas G. Rudawski ngr@ufl.edu (805) 252-4916 NOTE: this operating procedure assumes the user already has prior experience operating the instrument in STEM mode and has successfully configured and aligned the instrument for analytical work.

1. Getting started

1.1. Make sure you are in STEM mode and the probe is set and aligned for

analytical work (otherwise, it will be nearly impossible to generate a sufficiently large X-ray signal to perform meaningful EDS analysis).

1.2. On the EDS computer (left of TEM column), open the INCA © software .

1.3. Select “Project” in the “Navigator” tab and enter a project name and/or

info (a project may contain data for many samples); then select “Sample” and enter a sample name and/or info (optional)

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1.4. Under “Options” along the menu bar, select “Detector Control” (DO NOT open the shutter yet; the shutter should only be opened immediately prior to and during spectrum acquisition); leave “Detector Control” open during the use of the EDS system.

1.5. Under “Options” along the menu bar, select “Microscope Control”; leave “Microscope Control” open during use of the EDS system.

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2. “Analyzer” mode

2.1. At the bottom of the “Navigator” tab, select “Analyzer” . The analyzer mode acquires an EDS spectrum for a finite length of time while a live STEM image is acquired on the ASID monitor.

2.2. Select “Acquire Spectra” in the “Navigator” tab .

2.3. Open the detector shutter.

2.4. Select to start acquiring the spectrum (acquisition will stop automatically when the acquisition time has elapsed);

2.5. When acquisition has completed, immediately close the detector shutter.

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3. “Point & ID” mode

3.1. At the bottom of the “Navigator” tab, select “Point & ID” ; this mode acquires an EDS spectrum for a finite length of time (60 s by default) from specified points on a STEM image acquired in INCA ©.

3.2. Select “Image Setup” in the “Navigator” tab and enter in desired values for the STEM image acquisition; check “Enable SiteLock” direct the system to correct for drift (recommended).

3.3. Reopen the “Microscope Control” dialogue box and enter in the current STEM magnification (this needs to be done whenever the image magnification is changed; INCA © does not adjust it automatically).

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3.4. Select “Site of Interest” in the “Navigator” tab . 3.5. If spectra were previously acquired, create a new site of interest by selecting

; it is recommended to acquire only one spectrum per site of interest. Next, select to start STEM image acquisition; “BRIGHTNESS” and “CONTRAST” on the ASID may need to be adjusted until the image is visible when acquired in INCA ©; repeat image acquisition until satisfactory.

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3.6. Select “Acquire Spectra” in the “Navigator” tab .

3.7. Open the detector shutter.

3.8. Select and click on the desired location in the image (or use and click and drag) where a spectrum is to be acquired; acquisition will start immediately.

3.9. Immediately close the detector shutter after acquisition is finished.

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4. “Mapping” mode

4.1. At the bottom of the “Navigator” tab, select “Mapping” ; this mode acquires an EDS spectrum for a user-controlled length of time from specified line or box regions on a STEM image; the X-ray signals within the specific regions will be mapped within the STEM image.

4.2. Select “Image Setup” in the “Navigator” tab and enter in desired values for the STEM image acquisition; check “Enable SiteLock” direct the system to correct for drift (recommended).

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4.3. Select “Site of Interest” in the “Navigator” tab . 4.4. If spectra were previously acquired, create a new site of interest by selecting

; it is recommended to acquire only one spectrum per site of interest. Next, select to start STEM image acquisition; “BRIGHTNESS” and “CONTRAST” on the ASID may need to be adjusted until the image is visible when acquired in INCA ©; repeat image acquisition until satisfactory.

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4.5. Select “Smartmap” in the “Navigator” tab .

4.6. Open the detector shutter.

4.7. Draw (click and drag) a line or box tools to specify a region where X-ray mapping is to be performed (box shown here). Select to start mapping (acquisition will continue until is selected, so the acquisition time is arbitrary).

4.8. Immediately close the detector shutter after acquisition is finished.

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4.9. Select “Element Setup” in the “Navigator” tab . On the periodic table, select the elements to be mapped.

4.10. Select “Element Maps” in the “Navigator” tab to see the mapping of the X-ray signal for each selected element in relation to the acquired STEM image

(if a linescan was performed, select “Element Linescans” instead).

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5. Finishing using the EDS system

5.1. Verify that the detector shutter is closed.

5.2. Save your data and close INCA.