Measurement of trace samples

Fig. 1 shows the X-ray diffraction pattern and qualitative analysis results obtained by measuring a sample in which corundum (weight 0.2 mg) was placed on a non-reflective sample plate. Intensity sufficient for conducting qualitative analysis was attained with a measurement time of 1 minute or less.


Fig. 1: X-ray diffraction pattern and qualitative analysis results obtained from trace corundum

Fig. 2 shows the X-ray diffraction pattern for a trace amount of powder (weight 0.05 mg) obtained from a pill of Theodur, a type of medication for preventing asthma attacks. The qualitative analysis results confirmed the presence of anhydrous theophylline (the active ingredient) and lactose (the excipient). In this way, it is possible to quickly obtain the X-ray diffraction patterns necessary for identification, even with only a tiny amount of sample.


Fig. 2: X-ray diffraction pattern and qualitative analysis obtained from a trace pharmaceutical

Apparatus condition:

MiniFlex600 (F.F tube 40 kV, 15mA), Detector: D/teX Ultra

Measurement condition:

Al₂O₃: Slit conditions: DS = 1.25°, SS = 8 mm, RS = 13 mm, Incident side and receiving side Soller slit: 5°, Incident height limiting slit = 10 mm, Scan range: 2θ = 20 ~ 70°, Sampling step: 0.02°, Scan speed: 100° / min. (about 40 sec.)

Pharmaceutical drug: Slit conditions: DS = 0.1 mm, SS = 8 mm, RS = 13 mm, Incident side and receiving side Soller slit: 5°, Incident height limiting slit = 2 mm, Scan range: 2θ = 5 ~ 30°, Step width: 0.02°, Scan speed: 10° / min. (about 3 min.)


New sixth generation MiniFlex X-ray diffractometer (XRD) is a multipurpose analytical instrument that can determine: phase identification and quantification, percent (%) crystallinity, crystallite size and strain, lattice parameter refinement, Rietveld refinement, and molecular structure. It is widely used in research, especially in material science and chemistry, as well as in industry for research and quality control. It is the newest addition to MiniFlex series of benchtop X-ray diffraction analyzers from Rigaku, which began with the introduction of the original MiniFlex system decades ago. Read more...

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