X-ray Diffraction Calibration Procedures
Calibration of the X-ray Diffractometer will be performed a minimum of once per month.
However, calibration is not limited to once per month and can be performed as needed.
Load quartz standard slide into sample chamber.
Using “X-ray Diffraction Operation Guidelines”, acquire a diffraction pattern for the quartz
standard. For calibration purposes, ensure that the following variables are set as follows:
kV=30.0 mA=20.0
axes to scan: coupled
2 theta start = 5.0 2 theta end = 65.0 step size = 0.05 deg/min = 6.0
scan mode: continuous scan
The auto file ID should be named by typing “cb” followed by the numerical abbreviation for the
date on which the calibration is performed. For example if the calibration procedure is
performed on May 7, 2000 then the auto file ID should be named “cb050700".
Once the diffraction pattern is acquired, use “X-ray Diffraction Operation Guidelines” and the
“Materials Data JADE XRD Pattern Processing” manual in conjunction with the MDI JADE
5.0 software in order to identify the diffraction pattern. Use the Analyze and Find Peaks options
to locate major phases in the diffraction pattern (the default variables are suitable for finding
peaks). Use the Identify and Search/Match options to identify the diffraction pattern (search
the Inorganics Subfile - all other default variables are suitable for identification purposes).
Print the Search/Match hit list.
Print the diffraction pattern.
Staple these printouts together and file them in the XRD Calibration Folder.
Record the date, calibration standard, search/match results, and user initials in the XRD
Calibration Log.
NOTE: “X-ray diffraction Operation Guidelines”, “Materials Data JADE XRD Pattern
Processing” manual, XRD Calibration Log and Folder, and other XRD reference materials and
Logs are located at the XRD user station
X-ray Diffraction Calibration Procedures
Calibration of the X-ray Diffractometer will be performed a minimum of once per month.
However, calibration is not limited to once per month and can be performed as needed.
Load quartz standard slide into sample chamber.
Using “X-ray Diffraction Operation Guidelines”, acquire a diffraction pattern for the quartz
standard. For calibration purposes, ensure that the following variables are set as follows:
kV=30.0 mA=20.0
axes to scan: coupled
2 theta start = 5.0 2 theta end = 65.0 step size = 0.05 deg/min = 6.0
scan mode: continuous scan
The auto file ID should be named by typing “cb” followed by the numerical abbreviation for the
date on which the calibration is performed. For example if the calibration procedure is
performed on May 7, 2000 then the auto file ID should be named “cb050700".
Once the diffraction pattern is acquired, use “X-ray Diffraction Operation Guidelines” and the
“Materials Data JADE XRD Pattern Processing” manual in conjunction with the MDI JADE
5.0 software in order to identify the diffraction pattern. Use the Analyze and Find Peaks options
to locate major phases in the diffraction pattern (the default variables are suitable for finding
peaks). Use the Identify and Search/Match options to identify the diffraction pattern (search
the Inorganics Subfile - all other default variables are suitable for identification purposes).
Print the Search/Match hit list.
Print the diffraction pattern.
Staple these printouts together and file them in the XRD Calibration Folder.
Record the date, calibration standard, search/match results, and user initials in the XRD
Calibration Log.
NOTE: “X-ray diffraction Operation Guidelines”, “Materials Data JADE XRD Pattern
Processing” manual, XRD Calibration Log and Folder, and other XRD reference materials and
Logs are located at the XRD user station
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