Bulk sample measurement: Paper

Powder X-ray diffractometers can readily measure bulk samples provided techniques are devised for sample preparation. In the case of samples in sheet form, such as paper or film, a diffraction pattern with no angular error can be obtained, as shown in Fig. 1, by: (1) Cut the sample to the same size as the aluminum sample plate, (2) Stacking the sample and sample plate, and (3) Set the sample plate into the sample clip. If the sample has enough rigidity and thickness, it should be placed directly onto the sample clip, without using the aluminum sample plate.

Fig. 1: Preparation of samples in sheet form

Fig. 2 shows the X-ray diffraction pattern for two types of paper (magazine, white envelope). It is evident that both samples contain cellulose (the main component of paper), but each has different materials, such as clay minerals (e.g., kaolinite), calcium carbonate (calcite, aragonite) and titanium dioxide (rutile, anatase), which are used for surface treatment.

Fig. 2: X-ray diffraction pattern of paper

Apparatus condition:

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

Measurement condition:

Scan range: 2θ = 5 ~ 55°, Step width: 0.02°, Scan speed: 20° / 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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