X-ray diffraction (XRD) analysis of Ammonium Metatungstate is an important means of determining its properties such as crystal structure, lattice constant and phase purity. The following are the detailed steps for performing XRD analysis of Ammonium Metatungstate:
- Preparation
Safety check
Ensure the safety of the laboratory area by using personal protective equipment such as laboratory clothing, gloves and goggles.
Sample Preparation
Obtain a representative sample from the Ammonium Metatungstate product and ensure that the sample is dry, pure and uncontaminated. For XRD analysis, the sample should normally be in powder or single crystal form.
- Sample Loading
Place the sample on the XRD table, making sure that the sample surface is smooth and flat. If the sample is in powder form, a glass slide or other suitable carrier may be used.
- Adjusting the X-ray diffractometer parameters
Selection of X-ray source
According to the nature of the sample, select an appropriate X-ray source, usually the copper (Cu) Kα line (wavelength λ = 1.5406 Å).
Setting the scanning angle
Set the scanning range and step angle of the X-ray diffractometer. For ammonium metatungstate, the usual scanning range may be from a few degrees to a few tenths of a degree, and the step angle may be 0.01° or 0.02°.
Calibration
Perform calibration of the instrument to ensure that the X-ray diffractometer is in good working order.
- Making X-ray diffraction measurements
Start the X-ray source
Start the X-ray source and wait for it to stabilize.
Start scanning
Start the X-ray diffraction scan and record the diffraction pattern of the sample at different angles. This process can take anywhere from a few minutes to several tens of minutes, depending on the scanning range and stepping angle.
- Data processing
Analyzing Diffraction Patterns
The obtained pattern is analyzed using X-ray diffraction software to identify the diffraction peaks. These peaks correspond to different crystal structures or phases in the sample.
Determination of lattice constants
The lattice constants are calculated using Bragg’s law to obtain information about the crystal structure of the sample. For ammonium metatungstate,,it belongs to cubic crystal system with cell parameter α = 18.08 Å.
- Interpretation of results
Analyze the diffraction peaks
The position, intensity and shape of the diffraction peaks are analyzed to understand the crystalline nature of the sample. For ammonium metatungstate, the type of crystal structure and phase purity can be determined from the position of the diffraction peaks.
Determination of crystal structure
Using the diffraction data, determine the crystal structure of the sample, including the lattice type and cell parameters.
- Shutting down the X-ray diffractometer
Stopping the measurement
After completing the X-ray diffraction measurements, stop the X-ray diffractometer. Turn off the X-ray source and other related equipment, and disconnect the power supply.
Precautions
Ensure that the X-ray diffractometer is in proper calibration before performing experiments. Follow laboratory safety regulations and use personal protective equipment. Select the appropriate X-ray source and instrument parameters according to the nature of the sample.
X-ray diffraction analysis of ammonium metatungstate is a systematic process involving steps such as sample preparation, loading, parameter setting, measurement, data processing and interpretation of results. Through this process, detailed information about the properties of ammonium metatungstate such as crystal structure, lattice constant and phase purity can be obtained.
More details of ammonium metatungstate product, please visit website: http://ammonium-metatungstate.com/
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