Setup: Quatitative Analysis

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Quantitative Analysis

From the main SX-100 toolbar, LC QUANTITOOL. A quantitool window will open. This takes up to a minute.
On the left-hand side of the QUANTITOOL icon, LC BULK
From the QUANTITOOL window, LC CALIBRATE.
Make a list of the elements that you want to calibrate, decide on the standard, crystal, background positions and slope factors that you will need to use. In order to do this, you can use the UTILITY tool. To access UTILITY, from the QUANTITOOL window, LC UTILITY. Under FILES, select "calib WDS Peak-Background". You will now see a list of previously-done calibrations for specific elements. Use these to give you an idea of how to proceed with your calibration. Also, you can use the list of standards in the "standards" section of the instruction binder to help decide which standards and reference materials may be useful. Keep in mind that to save time, you can calibrate more than one element on a single standard.

Calibrating

Decide which element to do first, and in the CALIBRATE tool, choose the appropriate standard.
Deselect the spectrometers that you do not need.
To select standard, RH on the arrow next to STANDARD. Select the standard that you want.
Select the appropriate accelerating voltage (normal 15 kV), and appropriate probe current (usually 20 nA)
RH on the CONDITION line. Select "Recall calib" and then slide right to choose the appropriate setup for the element that you want to calibrate.
LC ACQUIRE. Once the stage moves to the standard, optically focus the sample using the Z wheel. When message "Adjust column and stage conditions" appears, LC OK.
A peak search will take place now. When the peak search is done, verify that the peak looks OK by opening the WDS window, and looking at the display. If peak looks OK, LC OK when you get the "Verify Peak Position" message
When you get the "Set PHA" message, LC YES
When message appears "Adjust Stage for Measurement", move the stage slightly and refocus using the Z wheel. FOCUS VERY CAREFULLY!!! When done, LC READY.
Counting will begin. At least 3 peak and background counts must be done on the standard, and you will be cued to move the stage each time. You must LC OK when a new position is selected.
Do enough count cycles so that the "meas. dev." is equal to, or less than, the "theo. dev."
Once the "meas. dev." is similar to the "theo. dev.", LC "stop calib"
Next, you have a chance to remove any counts that you don't want. LC "confirm" to go ahead and remove counts.
LC STORE when done.
Go through this process for all standards

PREPARING the DEFINITION FILE.

Set up DEFINITION for analysis. This selects that elements that you want to analyze, sets the analytical conditions and the order of analysis.

On the QUANTITOOL bar, LC DEFINE.
RH TYPE- select GEOLOGIC
RH SPECIES- select appropriate species.
LC LABEL. Change the label to a unique identifier. But, you must keep the first 4 letters of the name. For instance OLIV-7411 could be a label for olivine analysis set up on April 11, 1997. An alternative approach is to label the file with the beam size, such as OLIV-10 for an olivine file with a 10 micron beam.
Set accelerating voltage. Usually 15 kV
Set probe current. Usually 20 nA.
Select beam size on the COLUMN window.
RH APPEND and select elements that you want to analyze in order of increasing Z. If you make a mistake, you can use the "DELETE" and "INSERT" commands.
Select beam size on the COLUMN window.
Go to scanning mode and increase the magnification to a high value.
Return to FIXED PROBE mode.
When done, LC STORE.

Updating a DEFINE file

The "DEFINE" file saves all of the instrumental conditions at the time that it is saved. Therefore, before starting an analytical session, you need to re-open and re-store the DEFINE file.

RH LABEL, choose appropriate label.
If necessary, correct the number of oxygens, and the number of H₂0 (particularly if you're using "misc")
Make sure that the beam current, HV, and beam size are set correctly on the BEAM SETUP panel
Set scanning magnification to a high value
If you've recalibrated any element, and want to incorporate the new calibration information in your file, go to UTILITY and see if the old calibration file, and the new one both exist. If not, the information in the old and new were sufficiently similar that the old one was automatically overwritten by the new. Identify the files that you want.

To proceed with an individual spot analysis in single point mode (not actually used much, but try this first to get used to the steps that you'll need to follow on a regular basis).

LC ANALYZE on the QUANTITOOL tool bar.
RH ACQUIRE
Select GEO SINGLE POINT.
RH CURRENT area. Select appropriate current.
RH in the LABEL area. Select the appropriate label.
Add comment.
LC CONTINUE
Find the spot that you want to analyze using the optical microscope and/or BSE ( here you will need to switch from FIXED PROBE to SCANNING mode). I virtually always use BSE, and only use the optical microscope for the final optical focus
In BSE, with the beam on, increase the magnification until your analysis spot fills the entire screen
Blank the beam by putting in the Faraday cup.
***Optically focus*** in the SX-100 TV window, using the Z wheel. You'll have to turn the light on if you've just been in BSE. BE SURE TO NOT FORGET THIS STEP.

For the next point, continue from step 5.

To store points in XYZ

This is the more typical format to use for quantitative analysis. You can store a large number of individual points, line scans or gridded points, and the probe will run them for you automatically.

LC XYZ in the QUANTITOOL window.
Decide if you want to program points, line scans or grids. Select the appropriate choice. The following instructions are for POINTS.
If in the lower right corner of the XYZ window, the line has a number higher than 1 associated with the number of points, RH DELETE, and select DELETE ALL.
Find the spot that you want to analyze using the optical microscope and/or BSE ( here you may need to switch from FIXED PROBE to SCANNING mode, depending on what was being done last). I virtually always use BSE, and only use the optical microscope for the final optical focus
In BSE, with the beam on, increase the magnification until your analysis spot fills the entire screen
Blank the beam by putting in the Faraday cup.
***Optically focus*** in the SX-100 TV window, using the Z wheel. You'll have to turn the optical light on if you've just been in BSE. BE SURE TO NOT FORGET THIS STEP.
RH on the bar next to LABEL, and select the label that is appropriate for the spot that you've selected for analysis.
Put in a unique comment for this analytic point
LC ADD
You can see all of your saved points by opening VIEW.
Record the point in your lab book and sample map. In my lab book, I normally record the analysis point number, the label file, the sample name and point number, and then some comments about the spot.
To save the next point, go back to step e and start there.
Once all of your points are stored, LC DONE.

RUNNING YOUR STORED POINTS AUTOMATICALLY.

Once you've stored in all of your points, you can have the SX-100 run them automatically while you go off and do something else. Very convenient! There are two ways to doing this, either Geo Multipoint acquisition, or acquisition from within TASK. Geo Multipoint is easier, but does not have the ability to turn off the beam when acquisition is done. I almost always use TASK.

*** BEFORE *** starting an automated analytical run, you should always verify the spectrometers. To do this, go to STEP 9 in the "GETTING STARTED" instructions, and go through the steps described there.

Using TASK.
1. LC TASK from the SX100 icon bar.
2. Delete any tasks on the list
3. RH QUANTI, select xyzpos.dat (or line, or grid file)
4. If you want the beam to turn off when the acquisition is complete (for instance, an overnight run) RH TASK, select stop.tsk Now xyzpos.dat and stop.tsk should both be on the list, with xyzpos.dat first.
5. LC START
Using Geo Multi Point
1. In the QUANTI window, select ANALYZE
2. Select ACQUIRE
3. Select GEOMULTIPOINT
4. That's all.

Storing and printing data

Once you're done with a set of analyses, you will want to print the data, and also store the data in a format that you can access using a spreadsheet program.

You will need to store the data after:

1. Finishing a set of "Geo Single Point" analyses

2. Finishing a single XYZ multipoint run, either run by TASK or GEOMULTIPOINT

THIS IS VERY IMPORTANT!! If you do not store the data, it will be overwritten by the next set of analytical data.

Storing the master file for analyses obtained in Geosinglepoint or Geomultipoint.

Hold down the RM button within main window that contains all of the data.
Select FILE, then STORE AS NEW FILE.
Type in your directory, type in the filename, and click STORE

Storing the master file from TASK.

Hold down the RM in the window area.
Select HISTORY
Slide right
Select STORE LOG AS NEW FILE
Type in a filename. The directory cannot be changed at this point. Use the file manager to move this file to your home directory.

Storing and printing the individual label files.

Once you've done the previous step, all of your raw and processed data is safely stored. Now, you can use the REPORT tool to print your data in a nice format and also to save your data to a file in a format that can be read by Excel, or another spreadsheet.

On the open QUANTI menu, LC BULK on the PROCESS side of the window. A window called Quanti Process will open.
LC REPORT in the lower right corner.
RH on NAME, select the label of the file that you want to print or save as a file You must make separate reports for each label used, ie. FELD, PYRO, OLIV, etc...
Now you can experiment with different scripts, which will give you different output formats. You can view the output on the screen when the device selected is SUNDISPLAY
To print you output, change the device to LINEPRINTER, select the script that you want, and LC REPORT.
To save your output as an ascii file, change the device to FILE, select the script that you want, change
format from UNIX to DOS, select your directory, type in a filename, and LC SAVE.

If you want to print data, I would recommend using a script that includes the ID label of individual analyses (such as NORMAL or SIMPLE). The script titled COMPOUND-COLUMN is a convenient format for importing the data into a spreadsheet. I would recommend printing data AND saving data to a file.

Moving the files from the SUN to your computer using FTP.

Be sure that the black cable is plugged into the wall. This cable is located near the printer.
Work in the console window.
Change into your directory using the cd (change directory) command. If you need to move up a directory, use the command "cd ..". If you need to move down a level, type cd "new directory name" (cd Quanti). The case must be correct.
From within your directory, you will want to ftp to another computer. For instance, to ftp to "black.nmt.edu" type ftp black, then hit return. You should be prompted for a username and password that you will need to supply.
Once you are logged in, type bin to change the transfer mode to binary.
type mput *.* Then, you will be prompted, file by file, during the transfer. Answer yes to the prompt if you want the file to be transferred, and answer no if not.