eTraining Introduction How to Use This Module Introduction Choosing the Preparation Method Mount Fabrication Procedure Steel Etching Procedure Steel Polishing Procedure Rocks and Minerals Equipment Procedure Introduction Jet Spraying Lofting Suspension Odd Shapes - Fractures Cryo Fracture Technique Electronic Materials and Carbon Nanotubes Multiprep Polishing Procedure Handling Specimen Coating Reasons for Coating Metal Coating Procedure Carbon Coating Procedure Introduction Specimen Holders by Instrument Overview Interactive Parts Tour Operating Procedures Overview Chemicals and Materials Solution Preparation Chemical Calculations Fixation and Dehydration Mounting Safety and Disposal References Form and Function Signal Source and Detection Interactive Parts Tour Interactive Cutaway Tour Safety Procedures Operating Procedures Basic Imaging Advanced Imaging EDS X-Ray Spectral Analysis EDS X-Ray Mapping WDS Quantitative Analysis Procedure WDS X-Ray Mapping Overview WDS X-Ray Mapping Procedure Shut Down FAQs Troubleshooting VIDEO: Specimen Loading Technique VIDEO: Start Up Technique VIDEO: Specimen Unloading Technique Form and Function 1 Form and Function 2 Chemical Analysis Interactive Parts Tour Interactive Cutaway Tour Software Tour Safety Procedures Preliminary Specimen Exchange Flashing Imaging Shut Down Backscatter Imaging Charging Specimen Types X-Ray Spectral Analysis X-Ray Mapping Why Use FESEM? Specimen Constraints General FAQs Troubleshooting X-Rays and Spectra Energy Dispersive Spectrometer Wavelength Dispersive Spectrometer Safety Procedures EDS Versus WDS Quantitative X-Ray Microanalysis Basic Science Interactive X-Ray Mapping Challenge FAQs Troubleshooting Overview Tapping Mode Laser Alignment Preliminary Alignment Operation Image Viewing/Offline Operation Shut Down Fluorescence Optical Microscopy Detection and Visualization Interactive Parts Tour Start Up Basic Operation Fluorescence Microscopy Shut Down Tips and Troubleshooting Interactive Parts Tour Start Up Basic Operation Fluorescence Microscopy Shut Down References System Requirements Alternative Content Contact General Lab Safety Disclaimers Usage Permissions Site Map

Microanalysis

EDS X-Ray Spectral Analysis

Prepare the Column

1. The working distance should be 39 mm, the default position.    
2. Set the accelerating voltage to achieve at least 2x over-voltage, usually 20 kV.    
3. Remember to turn off the infrared chamber camera.    
4. Insert the EDS detector into the chamber at 3.5 mm.    
5. Ready the SEM for point analysis by using either the spot mode or zooming to 300,000x on the region of interest.    
6. Focus on a speck of dirt or dust but NOT the area you are going to analyze. Focus the beam, then move to your analyzing area.    

Collect the Spectrum

Revolution Toolbar

Revolution Toolbar

The software and icons refer to the 4pi Revolution® software for Windows. Click the toolbar above for a larger view.

 

Revolution Icon1. Open the Revolution software on the computer. VIEW
2. Select File> New Catalog. This creates a “file drawer” for all of the spectra you wish to collect for a sample or specific condition. VIEW
3. Before collecting a spectrum, make sure that the Accelerating Voltage is correct. VIEW
4. Choose a Dwell Time of at least 60 seconds. VIEW
Camera Icon5. Select Acquire > Acquire Start or select the camera icon to begin collection. VIEW
6. Make sure the Dead Time is 25%-30%. Dead Time can be adjusted by using the Coarse and Fine Condenser Lens setting on the SEM. VIEW
Clear Icon7. Restart the acquisition by selecting the Clear (clr) icon.    
8. To manually identify elements, right-click in the spectrum area and select "Open KLMs". VIEW
Camera Icon9. To stop spectrum acquisition, select Acquire > Acquire Stop or select the camera icon. VIEW
10. Select Edit Manual to force the quant program to use only the elements in your spectrum. VIEW
Quant Icon11. Select the Quant (qnt) icon to perform quantitative analysis. VIEW

Save the Data

1. To give your spectrum a name, right-click on the spectrum and select "Rename Spectrum" or select Option > Rename Spectrum from the toolbar. VIEW
2. To retrieve your spectrum and quant data, select File > Export and choose the file format, usually JPG or TIF. VIEW
Quant Icon3. Turn off quant by deselecting the icon before acquiring a new spectrum. To collect a new spectrum, select File > New. VIEW
4. To add a new subdirectory, navigate to the “Users files” folder in the C drive. Create a new folder labeled with your first and last names within the “Users files” subdirectory.    
5. To save your spectra, select File > Save As. Navigate to your folder by selecting My Computer > C drive > Users files > your folder. VIEW
6. To view all of your collected spectra, use the scroll menu at the top right of the spectrum window. VIEW

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