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 System Requirements Alternative Content Contact General Lab Safety Disclaimers Usage Permissions Site Map

Microanalysis

X-Ray Spectral Analysis

Prepare the Column

Column Icon1. Select Analysis mode in the Column SetUp window. The working distance should be 12 mm, the default position. VIEW
2. Set the accelerating voltage to achieve at least 2x over-voltage, usually 20 kV.    
3. Remember to turn OFF the infrared chamber camera. VIEW
4. Insert the EDS detector into the chamber at 4.5 mm. VIEW
5. Focus properly and be sure to avoid cracks and contamination. Increase the magnification to 500,000 times.    

Collect the Spectrum

Revolution Toolbar

Revolution Toolbar

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

Revolution Icon1. Open the Revolution software on the Macintosh 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 Condenser Lens 1 setting in the Column SetUp menu. 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, open the "temporary user files" folder on the desktop and select the asterisk-like icon. Choose New Folder and make a folder entitled with your first and last names. VIEW
5. To save your spectra, select File > Save As. Navigate to your folder by selecting Desktop > temporary user files > your name and select Save. 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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