MiniFlex

Rigaku MiniFlex


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.

Advanced HPAD detector: 0D, 1D, and 2D modes
MiniFlex XRD system delivers speed and sensitivity through innovative technology advances, including the HyPix-400 MF 2D hybrid pixel array detector (HPAD) together with an available 600 W X-ray source and new 8-position automatic sample changer. This new direct photon counting detector enables high-speed, low-noise data collection and may be operated in 0D and 1D modes for conventional XRD analysis and 2D mode for samples with coarse grain size and/or preferred orientation. A variety of X-ray tube anodes – along with a range of sample rotation and positioning accessories, together with a variety of temperature attachments – are offered to ensure that the MiniFlex X-ray diffraction (XRD) system is versatile enough to perform challenging qualitative and quantitative analyses of a broad range of samples, whether performing research or routine quality control. The new (Gen 6) MiniFlex X-ray diffractometer system embodies the Rigaku philosophy of “Leading with Innovation” by offering the world’s most advanced benchtop XRD.

Powerful PDXL software is easy-to-use
Each MiniFlex comes standard with the latest version of PDXL, Rigaku's full-function powder diffraction analysis package. The latest version of PDXL offers important new functionality; including a fundamental parameter method (FP) for more accurate peak calculation, phase identification using the Crystallography Open Database (COD), and a wizard for ab inito crystal structure analysis.

MiniFlex X-ray diffractometer history
The Rigaku MiniFlex X-ray diffractometer (XRD) is historically significant in that it was the first commercial benchtop (tabletop) X-ray diffraction instrument. When introduced in 1973, the original Miniflex™ XRD was about one-tenth the size, and dramatically less expensive, than conventional X-ray diffraction (XRD) equipment of the period. The original instrument (Gen 1), and its successor that was introduced in 1976 (Gen 2), employed a horizontal goniometer with data output provided by an internal strip chart recorder. The third generation (Gen 3) instrument, introduced in 1995, was called Miniflex+. It provided a dramatic advance in X-ray power to 450 watts (by operating at 30kV and 15mA) and Windows® PC computer control. Both the Miniflex+ and the succeeding generation products employ a vertical goniometer and allow the use of an automatic sample changer. The fourth generation (Gen 4) Miniflex II instrument was introduced in 2006 and offered the advance of a monochromatic X-ray source and a D/teX Ultra 1D silicon strip detector. The fifth generation (Gen 5) MiniFlex600 system, introduced in 2012, built upon this legacy with 600W of available power and new PDXL powder diffraction software.

Overview
• New 6th generation design
• Compact, fail-safe radiation enclosure
• Incident beam variable slit
• Simple installation and user training
• Factory aligned goniometer system
• Laptop computer operation

Measurements:
• Phase identification
• Phase quantification
• Percent (%) crystallinity
• Crystallite size and strain
• Lattice parameter refinement
• Rietveld refinement
• Molecular structure

Options:
• 8-position autosampler
• Graphite monochromator
• D/teX Ultra: silicon strip detector
• HyPix-400 MF: 2D HPAD detector
• Air sensitive sample holder
• Travel case

MiniFlex



Benchtop X-ray diffraction (XRD) instrument
Qualitative and quantitative analysis of polycrystalline materials

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Video


MiniFlex Applications



Bulk sample measurement: Paper


Background

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.....






Checking molecular axis orientation through stretching



Background

In polymer materials processed into the shape of fibers or films, the molecular axes align in the direction of stretching. Therefore, when these types of material are measured, diffraction lines due to crystal faces in specific orientations are observed to be large (preferred orientation). By using this characteristic, and measuring while varying the placement of the sample relative to the scan axis, it is possible to investigate the direction of the molecular axes with respect to the material. In this case, the transmission method is used together with the reflection method. Here, we measured a PET film, both unstretched and stretched by 5 times, by mounting a general-purpose sample holder to a benchtop X-ray diffractometer and using the reflection method and transmission method.....




Bulk sample measurement: Tablet



Background

Powder X-ray diffractometers can readily measure bulk samples if techniques are devised for sample preparation, and measurement conditions are properly set. When measuring samples which have curved surfaces, such as pharmaceutical tablets and ball bearings, various effects are seen due to the curvature, such as shifting of the diffraction angle and widening of the full width at half maximum. In the case of samples with these kinds of surfaces, adjustment is done using clay or cellophane tape from the back side of the aluminum sample plate, so that the sample surface is at the same height as the reference surface of the sample plate. The effects of curvature can be reduced by performing the measurement while narrowing the divergence slit and the incident height-limiting slit. Fig. 1 shows the X-ray diffraction pattern and qualitative analysis results for a pharmaceutical tablet. As a result of measurement, it was possible to identify the active ingredients in the tablet as ibuprofen and ethenzamide.....




Chocolate or cocoa? X-ray diffraction: General comparisons


What do you think about when you hear the word chocolate? Yummy! Dark or milk? If you look at the back of your unsweetened/baking cocoa or chocolate you may expect to see cocoa or chocolate. Yes, but what else do you see? You may see "contains X% protein" or "Y% fat and fiber", perhaps more. Dietitians beware; this can significantly alter your caloric intake. Many people use the terms chocolate and cocoa interchangeably. Depending on whom you ask there may not be a difference, unless you've ever tried to substitute one for the other incorrectly while attempting to make your favorite chocolate cake. Other people will tell you that cocoa is made primarily from cocoa powder and chocolate contains more of the cocoa butter. People in the food and dietary industry know the difference and the importance of the distinction to maintain a quality product. X-ray diffraction (XRD) using the MiniFlex will easily illustrate the difference. Shown in the X-ray diffraction pattern overlay below, two distinct diffractograms are observed using the Jade software package. One is of baking cocoa and the other of baking chocolate from the same company at your local grocery store. Can you tell which one is chocolate and which one is cocoa?....






Composition of barite: A universal material


Background
Barite is primarily used in the oil drilling industry for lubrication of their drill bits during the drilling and cutting process. It is also used in a variety of other applications including pigments, inks, plastics and X-rays. The density and color of this natural mineral make this a valuable product. However, in each application the purity and composition of the contaminants should be closely monitored as it may alter the properties and function of the barite material. Shown in the provided diffractogram is a sample of barite collected on the MiniFlex. Using the Whole Pattern Fitting (WPF) program available in Jade, this material was identified to be 91.7% barite with contaminants of quartz and calcite....




Contamination makes aluminum oxide a priceless gem


Background

Aluminum oxide or corundum is a commonly available material. However, trace levels of contaminants in the crystal structure of aluminum oxide can result in priceless gems, such as rubies, sapphires, and emeralds. Rubies are corundum with chromium contaminants. It's the chromium that produces the deep red color. Next to diamonds, rubies are the most precious gems. Sapphires come in many different colors: yellow, red, pink, and the more traditional color, blue. The blue color is only possible when titanium and iron are both present in the structure....




Differences in intensity/resolution due to differences in X-ray tubes


Background
With the MiniFlex300/600, it is possible to select a fine focus tube (focal point size 0.4 x 8 mm²) in addition to a normal focus tube (focal point size 1 x 10 mm²) of the type generally used with powder X-ray diffractometers. Fig. 1 shows an overlay of diffraction peaks obtained by measuring with a normal focus tube and fine focus tube. Table 1 shows a comparison of intensity, and full width at half maximum (FWHM), which varies proportionally with resolution....




Differences in resolution due to differences in Soller slits


This application note demonstrates quantitative analysis for lubricating oil according to ASTM D6443-04 on Rigaku ZSX Primus, a wavelength-dispersive XRF spectrometer.
Background
The width of the standard incident and receiving Soller slits of the MiniFlex300/600 is 5°, but to obtain high-resolution it is possible to select a width of 2.5° (incident/receiving Soller slits) or a width of 0.5° (receiving Soller slit only). Fig. 1 shows a comparison of the X-ray diffraction profiles of LaB₆ powder when the Soller slit is changed, and Table 1 shows the intensity ratios, and the full width at half maximum (FWHM), which varies proportionally with resolution.




More application notes are available by submitting the application request form