4. Quick Reference Guide to Routine Calibration and Analysis

1. System Check
   1. Login to your account. If you don't see the login prompt, select Initialize Logout. Respond yes to the prompt. You should eventually see a login screen
   2. Open the Present Position monitor (Monitor Present Position). Check the following:
      1. Vacuum is ready
      2. Voltage is On
      3. There is a beam current
   3. The vacuum should be better than 6 x 10^-6 torr
2. Open Quantitative Analysis
   1. Previously existing Quantitative Setup
      1. Start the Quantitative program (Analysis Quantitative Analysis)
      2. Load your setup
         1. Sample Group Analysis Setup
         2. Load your condition file if it didn't load automatically. (Measurement Condition Load)
   2. New Quantitative setup
      1. Start the Quantitative program (Analysis Quantitative Analysis)
      2. Set up the analytical conditions you would like to use
         1. Select the correction routine you would like to use. (Measurement Correction Method) There are four choices:
            1. Oxide ZAF
            2. Metal ZAF
            3. Oxide PRZ (CITZAF)
            4. Metal PRZ (PAP)
         2. Set up the element conditions you want to use (Measurement Element Condition).
            1. Use the WDS Elements button to select the elements you want to use. (Select only the elements you want to analyze. Calculated elements are selected later)
            2. Click the WDS Conditions button to set up the measurement conditions. For each element you must specify the following
               1. X-ray Line (e.g. K, L)
               2. Order (Almost always 1)
               3. Channel (spectrometer) #
               4. Background offsets
               5. Measurement Mode.
                  1. Time. In this mode counts are collected for a fixed time
                  2. Counts. In this mode counts are acquired until a specified number of counts are collected.
               6. Peak Seek Width (Almost always 1)
               7. Measurement time or measurement counts, depending on which measurement mode you selected.
               8. The detector parameters (Items in gray) should not be changed.
               9. Spectrometer setups labeled with an asterisk should not be changed.
               10. NB. DO NOT USE READ OR SET BUTTONS.
            3. Click the CAL Elements button to select the elements you want calculated
            4. Click the CAL Condition button to set up the calculated elements. For most setups calculate oxygen as an anion. This is selected automatically when you select Oxide ZAF or Oxide PRZ.
         3. Set the EOS conditions you want to use for analysis (Measurement EOS Condition)
            1. Manually set the required voltage using the EOS Monitor (Monitor EOS Monitor).
            2. Set the required current using the probe current knob on the console
            3. Click the Read button on the EOS Condition window. Make sure Probe Scan is OFF, and that Probe Diameter is set to the desired value.
         4. Store the setup you have just created. (Measurement Condition Store)
3. Carry Out Calibration
   1. Start Calibration Program. (Analysis Standard Analysis)
   2. Carry out the following steps for each standard you will use
      1. Select the standard you want to calibrate (Measurement Sample)
      2. Check that Standard type is set correctly (Measurement Standard Type
      3. Set up the Spectrometer conditions for each element you are using in the standard (Measurement Element Condition). See section .B.2.b.2
      4. Set up the EOS Condition (Measurement EOS Condition). See section B.2.b.3
      5. Select analysis points
         1. Open the Stage Condition Input window (Measurement Stage Condition Position Input).
         2. Make sure the Stage button is selected.
         3. Set number of accumulations (Accumulation button). Usually four accumulations are used.
         4. Move to the standard using th Move button or the Stage Monitor (Monitor Stage Monitor)
         5. Select your first spot, focus and test
         6. Press the store button on the joystick keypad
         7. Press the confirm button, when the confirmation window opens press store to store your first point.
         8. Go to you next point, focus, test nd press store.
         9. Repeat for the remaining points
         10. Close the Stage condition windows
   3. Make sure that Print-out condition is ON (Measurement Print-out Condition).
   4. Run the calibrations
      1. Measurement Preset Conditions
      2. Clear old presets using the Clear button
      3. Select all the standards you have set up
      4. Press the Acquire button
   5. Check the results of the calibration
      1. For each of the standards check the following on the printout.
         1. Voltage and current are what you requested
         2. There is a significant net count rate
         3. Bg+ and Bg- are symmetrical (i.e. same order of magnitude
         4. S.V. / S.D. is less than 3
            1. If S.V. / S.D is greater than three you may still be able to use the calibration
               1. Open the Check Data window (Measurement Check Data)
               2. Click the ACM button, this will create a button on the accumulation column. Click this button
               3. Examine the list of count data, if there is one which is significantly higher or lower, click on it to remove it from the list
               4. Calculate S.V. ((sigma/net counts) * 100). If S.V./S.D. is less than three you can use the calibration, if not you must redo the calibration.
               5. Close the accumulation window, click the Save button and close the Check Data window
4. Check that the calibrations were picked up by the Quantitative Analysis program
   1. Check the Element Conditions (Quantitative Analysis Measurement Element Condition Condition)
      1. The Peak Position for each element should correspond to the one found in the calibration. If it doesn't , select the element and search the list for a matching peak position. If the setup is the same as the one you selected you can use this one
   2. Check Standard Conditions (Standard Condition)
      1. Each element in the list should have the name of the standard you want to use and today's date. If this isn't the case, click the button on top of the list and select the proper standard.
   3. Save the analytical condition (Quantitative Analysis Measurement Condition Store)
5. Select analysis points and carry out analyses
   1. Open the Stage Condition Input window (Quantitative Analysis Stage Condition Pos. Input)
   2. Repeat the following steps for all the required points
      1. Locate point of interest
      2. Focus and test the point
      3. Enter a comment
      4. Click the Read and Apply button
      5. Click the down arrow (upper right hand corner) to go on to the next point
   3. Close the Stage Condition window(s)
   4. Select printing ON or Off (Measurement Print-Out Condition
   5. Start the analyses (Measurement Preset Measurement Acquire

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