X-ray Diffraction Instructions
Operating Instructions for Philips X-Ray Diffraction Unit Using CuKa radiation and Scintillation Counter
Caution: When X-ray Fail Safe Light and Shutter Light are on, X-rays are in the sample chamber.
>Sample Loading Procedure
1. Check to see if shutter is closed and X-rays are off.
Sample Loading Procedure
1. Check to see if shutter is closed and X-rays are off.
2. Remove cover by loosening locking screw and pulling cover out and to the right.
3. Depress spring mechanism and place mount in chamber,
SAMPLE SIDE UP AND EXPOSED (not in the spring mechanism).
4. Replace sample chamber cover by aligning pin in hole
and pushing the cover back in while pressing the safety lever.
Tighten the screw gently.
Turning on the Diffractometer - Generator Panel
1. Check manual Selection for MA and KV: MA should be set at 10, KV at 25.
2. Under Display, check that MA mode and operate mode are illuminated.
3. Push the "X-ray On" button. Wait until MA display reads "9".
4. Slowly dial the MA to "20". Press the KV/MA button to read "KV".
5. Slowly dial the KV to "40". (Wait for each setting to appear on the LED.)
6. Depress shutter switch #4 until you hear a loud click and the red light goes on.
Turning off Diffractometer
1. Make sure the last scan parks the goniometer at 60o.
2. Depress shutter button 4 and make sure shutter light goes off.
3. Reset MA and KV to 10 and 25, respectively. (Slowly turn the dial.)
4. Press the "X-ray Off" button.
5. Remove slide as stated above and replace sample chamber cover.
NOTE: The equipment produces a hazardous primary X-ray beam.
NEVER TRY TO OPEN CHAMBER UNLESS YOU ARE SURE X-RAYS ARE OFF AND THE SHUTTER IS CLOSED!
Guide to Scanning and Interpretation of XRD Data
X-ray Diffraction Computer Instructions For Datascan 3.2 and Jade 7.0
The two programs of interest are Datascan and Jade.
Datascan is used to set the diffractometer parameters to collect a scan. It allows you to set a two-theta range, step speed, dwell time and a file path for your run. Jade analyzes the scan and identifies the minerals or compounds present. You may work with Jade on existing scan produced by Datascan while Datascan is collecting a new scan.
Log on to computer as “user.” Use "geochem" (all lower case) for the password. Log off via the Start button menu in the lower left of the screen.
Datascan:
Use the desktop icon to open Datascan.
Datascan
Scan
Setup - use "Default scan" for normal mineral scans
- Use pull down menu to select alternate scan parameters
Datascan
Scan
File – select file path - C:\Datascan\Data-jade\min04
- C\Datascan\Data02\Chem
- Or establish your own folder
Datascan
Scan – enter sample name for sample ID and file name
Start scan
When scan is finished you may print the scan directly from Datascan if no further analysis is needed. If doing further analysis in Jade delay printing and print from Jade.
Jade:
Use desktop icon to open Jade 7.0.
To open a pattern in Jade:
File
Patterns
Open C:\Datascan\Data-Jade\min04
Select pattern by double clicking on pattern name
To analyze a pattern opened in Jade and identify the minerals:
Analyze
Fit Background
Apply
Check Strip K-alpha 2 if strip desired
Analyze
Fit Background – this step removes background
Apply
Remove
Analyze
Find Peaks
Labeling
Select desired parameters (usually line marker and d-spacing)
Apply
Analyze
Find Peaks
Search
Apply
Identify
Search/match setup
Select database you wish to search – minerals, inorganics, superconductors, zeolites
Go
After selecting Go, Jade will perform Search/Match and present possible minerals in the pattern shown in the Search/March Display page. The lower the Figure of Merit -FOM - the greater the possibility the mineral is in the scan. FOM alone does not establish a match. To further analyze a pattern:
1) Select (by checking the box to the right of the mineral name) an individual mineral at the bottom of the display page. The positions of the peaks for that mineral will appear below the scan. Compare the pattern to the peak positions to determine if the checked mineral matches the pattern.
2) Select the mineral you believe matches the pattern. Determine if there is more than one mineral present by looking for pattern peaks that do not match a checked mineral. Clicking on the half moon icon at the top of the screen removes the selected mineral from the pattern and displays only the unmatched or residual peaks. If more than one mineral is present you may have to check several minerals to identify everything in the pattern.
3) Click the name or PDF number of a checked mineral. The database will provide a report of the d-spacing for that mineral. Compare this report to the report you printed of the measured peaks.
Once you have decided which mineral (or minerals) produced the pattern press escape esc on the keyboard. You may now print your final report:
Identify
Search/Match Report – select parameters
Print
If you need to return to the Search/match Display page for further analysis–
Identify
Search/Match Display
Remember to turn X-rays off and to log out of computer.
