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SOP for XRD by using X'pert Highscore Plus (Basic)

Method · January 2014

DOI: 10.13140/RG.2.1.3940.5042

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 SOP
(Standard
X-RAY DIFFRACTION
Operation
Procedure)
Analytical Laboratory, Faculty of Engineering

STANDARD OPERATION PROCEDURE

(SOP)

X-RAY
DIFFRACTION
(For Analytical Unit usage)

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X-RAY DIFFRACTION SOP REV1.0
(PIC Fareez)
 SOP
(Standard
X-RAY DIFFRACTION
Operation
Procedure)
Analytical Laboratory, Faculty of Engineering

X-RAY DIFFRACTION SOP REV1.0

PRINCIPLE:

X-ray diffraction is a technique most commonly applied to materials which are crystalline in the
solid state. It is unsurpassed in its ability to provide three-dimensional structural information. It
provides information on the arrangement of molecules or other structural units as well as on
local structure.

APPLICATIONS:

 Identification of known materials and phases from their diffraction patterns

 Identification and characterisation of new materials
 Determining precise molecular structure, connectivity and geometry
 Establishing the absolute configuration of chiral compounds
 Determining the extended structures of materials
 Studying non-crystalline materials
 Observing changes in structure as a function of temperature, pressure, magnetic field,
illumination or amount of reactant

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X-RAY DIFFRACTION SOP REV1.0
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 SOP
(Standard
X-RAY DIFFRACTION
Operation
Procedure)
Analytical Laboratory, Faculty of Engineering

I. INSTRUMENT SAFETY

The X-Rays On light on top of the diffractometer is your first safety indicator; it is lit when the
generator is turned on. The front control panel includes additional safety and instrument status
indicators. A close-up of the front control panel is shown in Figure 2.2. The enclosure doors are
leaded so that they are radiation shielding. Before the shutter can open, these doors will lock—
thereby preventing you from entering the enclosure when there is a danger of exposure.

Figure 2.1

The enclosure for the

X’Pert Pro MPD

Figure 2.2 The front control panel for the X’Pert Pro MPD.

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X-RAY DIFFRACTION SOP REV1.0
(PIC Fareez)
 SOP
(Standard
X-RAY DIFFRACTION
Operation
Procedure)
Analytical Laboratory, Faculty of Engineering

PROCEDURE:

1. (INSTRUMENT - START)

1. On the chiller system.

2. Look at the Power On and HT indicator lights to determine if the generator is on.
a. If both lights are on, then the generator is on.
b. If both lights are off, then proceed to step 3
3. Make sure that the enclosure doors are closed.
4. Check if the HT indicator light on the front control panel is lit.
a. If it is, proceed to step 5.
b. If it is not, turn the HT key (above the HT light) clockwise.
i. The HT indicator should light up.
ii. Proceed to step 4.
5. Press the Power On button on the front control panel.
a. If everything works properly
i. The Standby indicator light will turn off
ii. The Power On indicator will light up
iii. The system will start an initialization process.
iv. The tube power will be turned to 30 kV and 10 mA
v. The tube and detector will be moved to their starting positions
vi. The diffractometer is now on.

2. (SOFTWARE)

1. Start X’Pert Data Collector.

a. Either double-click on the desktop icon, double-click on the Quick Launch icon, or select
the shortcut in the Start Menu> Programs> PANalytical> X’Pert Data Collector.
2. Enter the user name and password and press .
a. The current password for all users is soap
3. In X’Pert Data Collector, select Instrument> Connect.
4. Choose the correct configuration for your sample stage.
5. Press .

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X-RAY DIFFRACTION SOP REV1.0
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 SOP
(Standard
X-RAY DIFFRACTION
Operation
Procedure)
Analytical Laboratory, Faculty of Engineering

3. (CHANGING THE TUBE POWER) – BREEDING

1. Go to the Instrument Settings tab in the Instrument Window.

2. Double-click on Generator.
3. If the Generator is off, then check the box next to “Generator On” and click Apply.
4. Press Breed  Select at normal speed  Press .

5. Wait around 30-60 minutes for X-ray tube to breed.

6. Once finish, then proceed to step 7.
7. Change the tube power
a. Change the values of “Tension (kV)” and “Current (mA)” to the desired values, and
then click on OK.
b. For the Cu tube
i. Collect data at full power:
1. “Tension”= 45 kV
2. “Current”= 40 mA
ii. When done, turn the power down to its
stand-by level:
1. “Tension”= 30 kV
2. “Current”= 10 mA

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X-RAY DIFFRACTION SOP REV1.0
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 SOP
(Standard
X-RAY DIFFRACTION
Operation
Procedure)
Analytical Laboratory, Faculty of Engineering

4. (SILICON CHECK)

1. Put the Silicon at Sample Stage.

Sample Stage

2. Select Measure  Program Select “SilicaCheck” parameter. Refer to item 5 (Scanning

Parameter – Sample)  Press .
3. Right click on the graph  See the value of first peak graph.
4. Silica peak check should be around 28.443 ± 0.04.
5. If the value in-spec then can proceed with the next sample.

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X-RAY DIFFRACTION SOP REV1.0
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 SOP
(Standard
X-RAY DIFFRACTION
Operation
Procedure)
Analytical Laboratory, Faculty of Engineering

5. (SCANNING PARAMETER - SAMPLE)

The parameters for this scan include:

File

o “Name”: the filename for the data file

o The default filename is a derivation of the program name
o The filename must be MS Windows legal.
 Do not use illegal characters such as / \ ? : * “ < > | % $ #

o “Folder”: the folder where the data will be saved.
o You can enter in the folder path

o Or you can click on the icon and navigate to the folder location
o “Comment”: this field is an optional page of description
o It will only be visible if you look into the raw data file text
o Sample description text, which will be visible in the header of data analysis software,
should be entered in the “ID” field, not the “Comment” field.
Sample

o “ID”: the is a description of the sample and measurement which will be displayed in header
or legend of data analysis software and reports
o It can contain any characters and be one line long
o “Name”: an optional sample designation that is not used by very many software packages
o “Prepared by”: optional field useful for tracking the person who created the sample or the
data
o “Name” and “Prepared by” fields are typically used in an industrial setting for QC
tracking
o They might be useful for your laboratory tracking too

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X-RAY DIFFRACTION SOP REV1.0
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 SOP
(Standard
X-RAY DIFFRACTION
Operation
Procedure)
Analytical Laboratory, Faculty of Engineering

6. SAMPLE ANALYSIS

1. Start X’Pert Highscore Plus

a. Either double-click on the desktop icon, double-click on the Quick Launch icon, or select
the shortcut in the Start Menu> Programs> PANalytical> X’Pert Highscore Plus.
2. Select the file that X’Pert Data Collector has produced in same folder.
(.xrdml format file)  Press .
3. Select “Treatment”  Select “Determine Background”. Press Background  Press Accept.

4. Select “Treatment”  Select “Smooth”. Either Cubic or Quintic. This is to eliminate the noise
that produced during sample analysis. *Level of Convolutions range can be change depend
on the result produced.

5. Select “Treatment”  Select “Search Peaks”

6. Set “Minimum significance” to 4.00 (Depend)  Select “Search Peaks”  Select “Accept”.

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X-RAY DIFFRACTION SOP REV1.0
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 SOP
(Standard
X-RAY DIFFRACTION
Operation
Procedure)
Analytical Laboratory, Faculty of Engineering

7. Select ‘Analysis”  Select “Search & Match”  Select “Execute Search & Match”

8. If there no any restrictions of elements, then press .

9. If the sample has restrictions of elements, Select ‘Edit Restrictions Sets”  Select “Periodic
Table”  Choose your element that you want to focus.

Note:
User can choose certain
element in Periodic Table
which is related with
sample that has been
analyzed. It could help
the user to find the exact
pattern in ICSD library

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X-RAY DIFFRACTION SOP REV1.0
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 SOP
(Standard
X-RAY DIFFRACTION
Operation
Procedure)
Analytical Laboratory, Faculty of Engineering

10. Choose the highest score  Drag it to “Accepted. Pattern”

11. Select ‘Reports”  Select “Word Report”  Select “Fancy”

12. Report produced.

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