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