
D2 PHASER 2nd Generation
Take a look under the hood of the world fastest X-ray benchtop diffractometer.
Take a look under the hood of the world fastest X-ray benchtop diffractometer.
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What do you obtain when patented technologies, award-winning software, a fully functional PC with monitor and state-of-the-art detectors meet up with leadership in innovative X-ray diffraction? Perfect solutions for powder diffraction. And if it all fits onto a table, it is called: D2 PHASER! What enables this evolutionary leap to take place and how can the amazing performance of this space saving sensation actually be explained? First of all, you develop an ultra compact goniometer, file a patent, complete the system with all the other components for autonomous operation and package the whole configuration together with a fully functional PC, monitor, keyboard and mouse, into a compact housing. Second, you use the unique DIFFRAC.SUITE software for controlling the instrument and analyzing the data. Since its introduction the DIFFRAC software has developed into a high performance tool for the characterization of crystalline phases in research and industry. Third, you use only the best components, for example the LYNXEYE detector. This state-of-the-art and extremely efficient 1-dimensional detector simultaneously captures a large angular range and radically reduces the measurement time: hours turn into minutes. Combining all of these innovations creates a benchtop X-ray diffractometer which has the analytical performance and functions of a large instrument, but which is easy to transport and opens up the whole world of powder diffraction without a lot of infrastructure. D2 PHASER – never before was benchtop X-ray diffraction better, smaller and more powerful! |
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Wishes come true – comprehensive, unique and non-destructive characterization of crystalline samples by means of X-ray diffraction (XRD) with the D2 PHASER. Our D2 PHASER opens the door to modern XRD for you. This means qualitative and quantitative phase analysis, polymorphism investigation, the determination of crystallinity, all the way through to structure investigation – all of it fast, simple, efficient and with high quality. It is not just its analytical performance that makes the D2 PHASER so revolutionary, but also its flexibility in handling very diverse samples. Different material properties require different sample preparations. Therefore, besides a series of standard sample holders made from PMMA or steel, the D2 PHASER also offers holders for small sample amounts, low-absorbing and weakly diffracting samples, for filters, for environmentsensitive samples and for examining materials that tend to show a preferred orientation. LYNXEYE XE-T fast-lane edition What makes the D2 PHASER absolutely unique is the integration of the world's leading 1-dimensional detector for X-ray powder diffraction: Our LYNXEYE XE-T. With a performance enhancement in terms of intensity by a factor of more than 450, the D2 PHASER is actually playing in the top class. Additionally the LYNXEYE XE-T allows suppression of sample fluorescence providing an excellent peak-to-background ratio even for strongly fluorescent samples, eliminating any need for secondary monochromators and makes Kß-filter redundant. D2 PHASER XE-T edition – X-ray diffraction in a new dimension! |
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Holders with various cavities |
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Holder for automated sample preparation. |
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Holder for clays |
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Low back ground holders for small sample amounts |
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Airtight holders for environment sensitive samples |
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Holder for filter samples |
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Can XRD – the best method for phase characterization – really produce high quality data without the need for a corresponding infrastructure? Yes! With our D2 PHASER a new era begins. All that is required is a simple domestic wall socket and you can start producing outstanding analytical results: Plug ‘n Analyze. Since it is a desktop system it requires only a minimum amount of space and is in no way inferior to a large system in terms of its analytical performance. Resolution, angular accuracy and data statistics set new standards in this class of analytical instruments; data quality which you can rely on and with which even complex questions can be answered. Our D2 PHASER is a transportable all-in-one instrument that requires no additional cooling water or PC peripherals. This means that there is nothing to prevent it from being used outdoors: simply switch-on a power generator, plug in the connector and start measuring! Our D2 PHASER is fully network capable. This enables XRD experts in the central laboratory to access the data that has been collected, no matter if they are next door or at the other end of the world. Use the D2 PHASER where it is needed – on-site – and you will save time and money! D2 PHASER – X-ray diffraction tool for everyone – everywhere! Get more information on www.bruker.com. |
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Cement & Raw Materials |
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Minerals & Mining |
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Geology & Exploration |
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Ceramics |
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Chemistry & Catalysts |
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Research & Education |
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Pharmaceuticals |
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Environment |
The D2 PHASER is a portable desktop XRD instrument for research and quality control. It is easy to operate and independent of external media such as cooling circuits. Thanks to the LYNXEYE detector it is the fastest desktop XRD system on the market. This report demonstrates its use for fast and reliable phase identification. X-ray powder diffraction is a fast method for determining the phase content of polycrystalline material. Every material exhibits a typical ‘X-ray fingerprint’, which is stored in databases such as the ICDD PDF2 or PDF4. This fingerprint is utilized in the DIFFRAC.EVA software for phase identification. Furthermore, automatic scaling of the patterns from the database relative to the measured intensities gives the semi-quantitative phase composition. |
Pulverized geological material was measured with the D2 PHASER. Experimental details are summarized in Table 1. Figure 1 shows a zoomed region (intensities are cut at about 10% of the maximum intensity) of the diffraction data together with the result of the phase identification. The data, collected within 45 minutes, show a very good counting statistics. Minor phases of less than 1 wght-% are clearly identified. Using the D2 PHASER the value of the investigated geological sample for use in building materials could immediately be shown. |
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D2 PHASER Desktop XRD |
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Holders with various cavities |
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LYNXEYE 1-dimensional detector |
The D2 PHASER is a portable desktop XRD instrument for research and quality control. It is easy to operate and independent of external media such as cooling circuits. Thanks to the LYNXEYE detector it is the fastest desktop XRD system on the market. This report demonstrates its use for quick and reliable crystallite size determination. X-ray powder diffraction is a fast method for determining the average size of crystallites. The crystallinity of petroleum coke (expressed as Lc value) is a measure of quality affecting suitability for the end use of the coke, and is a function of the heat treatment of the coke. The ASTM norm D 5187 describes how to obtain the crystallinity of coke by evaluating the shape of a carbon X-ray peak. This peak is scanned over a wide range and the Lc value calculated from the full width of the X-ray peak at half maximum intensity. |
A coke powder specimen was prepared according to ASTM D 5187 and measured with the D2 PHASER. Experimental details are summarized in Table 1. Figure 1 shows a typical diffraction scan from petroleum coke. After automatic subtraction of the base line, DIFFRAC.EVA estimates the crystallite size by means of the Scherrer equation from the full width of the peak at half maximum. The data presented in figure 1 exceeds the maximum peak intensity (in cps) shown in ASTM D 5187 by a factor of 50. Notably, this data was collected in less than 1 min, compared to 20 min mentioned in the norm. The 1-dimensional LYNXEYE detector makes this intensity and speed gain possible, even for a low powered XRD system. To conclude, our cost-effective desktop XRD system D2 PHASER allows for extremely fast and precise quality control of anode coke material. |
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D2 PHASER Desktop XRD |
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LYNXEYE 1-dimensional detector |
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Holders with various cavities |
The D2 PHASER is a portable desktop XRD instrument for research and quality control. It is easy to operate and independent of external media such as cooling circuits. Thanks to the LYNXEYE detector it is the fastest desktop XRD system on the market. This report demonstrates its use for monitoring occupational exposure to respirable silica. Lung cancer and other health issues are known to be associated with occupational exposure to crystalline silica, SiO2. This is a typical component of soil and rocks. Clear exposure/response relations were reported for e.g. miners, diatomaceous earth and construction workers, granite, pottery, refractory bricks, or foundry workers. Occupational exposure to respirable silica is a preventable health hazard and therefore, the concentrations are monitored. X-ray powder diffraction is capable of distinguishing polymorphs of crystalline silica (quartz, cristobalite, tridymite). Furthermore, XRD may account for the interference with other minerals that may additionally be present at the workplace. Sampling of the airborne particles on filters and their investigation is regulated by several national norms like NIOSH 7500, OSHA ID-142, MSHA P-2, and others. The concentration of an unknown silica phase is determined from a calibration, which needs to be established from reference samples using e.g. the DIFFRAC.DQUANT software. |
Filter papers with different amounts of quartz deposited were measured applying the D2 PHASER and a special sample holder for filters. Experimental details are summarized in Table 1. Figure 1 shows several diffraction scans of the 100% quartz peak. The different intensities are directly related to the concentration of the deposited quartz dust. The net intensities of the different specimens show a clear linear correlation with the concentrations (see inset). The calibration fully complies with the NIOSH norm. The curve has zero offset of 2.7 µg (±5 µg permitted in NIOSH 7500). The limit of detection (LOD) in this example is about 8 µg. It can further be reduced by increasing the measurement time. A counting time of 5 sec per step for example, increases the total scan time to about 25 min but reduces the LOD below 5 µg. The precision is better 1 % relative for concentrations exceeding 100 µg and better 10% relative between 10 and 100 µg. To conclude, our cost-effective desktop XRD system D2 PHASER allows for fast, precise and norm compliant analyses of airborne respirable silica particles on filters. |
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D2 PHASER Desktop XRD |
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LYNXEYE 1-dimensional detector |
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Holder for filter samples |
The D2 PHASER is a portable desktop XRD instrument for research and quality control. It is easy to operate and independent of external media such as cooling circuits. Thanks to the LYNXEYE detector it is the fastest desktop XRD system on the market. This report demonstrates its use for investigating crystal structures applying the fundamental parameters approach in the TOPAS software. X-ray powder diffraction helps understanding the properties and the crystal chemistry of new tailor made materials of which no single crystals are available. This information can be accessed from the intensities of the diffraction peaks using the TOPAS software. Structural variations related to the substitution or Si and Ca against Al and trivalent Lanthanoid ions in the mineral melilite, a layered alumino-silicate with chemical formula LnxCa2-xAl[Al1+xSi1-xO7] 0≤x≤1 and Ln = La, Eu, Er, were recently studied [1]. They form solid solutions and are potential laser materials with interesting optical properties. |
About 10 mg Er-melilite of nominal composition x=0.5 were prepared on a low background Si sample holder and measured with the D2 PHASER. Experimental details are given in Tab. 1. The crystal structure, isotropic thermal displacement parameters of the atoms and the unit cell parameters were refined using DIFFRAC TOPAS v4. The fundamental parameters approach (FPA) was used for modeling the resolution function of the D2 PHASER. Figure 1 presents the TOPAS plot. Refined structural parameters are plotted vs. literature data [1] in the inset. The high data quality and the excellent refinement become obvious from the only minor deviations from linearity. From the cell parameters c/a ratio a composition of x=0.52 is calculated, in excellent agreement with the nominal value 0.5. The little residuum between calculated and measured data suggests that FPA perfectly models the measured peak shape of D2 PHASER data.To conclude, our cost-effective desktop XRD system D2 PHASER allows for fast, precise and norm compliant analyses of airborne respirable silica particles on filters. References: |
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D2 PHASER Desktop XRD |
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LYNXEYE 1-dimensional detector |
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Low back ground holder for small sample amounts |
The D2 PHASER is a portable desktop XRD instrument for research and quality control. It is easy to operate and independent of external media such as cooling circuits. Thanks to the LYNXEYE detector it is the fastest desktop XRD system on the market. The system delivers high quality measurement data, which allows performing advanced analytical methods, such as the standardless quantitative Rietveld phase analysis. This report demonstrates its use for the phase quantification of Ordinary Portland Cement Clinkers. X-ray powder diffraction combined with TOPAS Rietveld analysis is nowadays one of the most powerful methods existing, to perform quantitative phase analysis. In the last years it became a standard tool in cement industry for quality and process control, not only for clinker and cement analysis, but also for the whole process mineralogy. |
A clinker sample of the 2005 VDZ Round Robin (German Cement Works Association) was analyzed, to demonstrate the performance of the D2 PHASER for such applications. The measurement covered the angular range from 10 to 65° 2Theta. The scan time was about 25 minutes. Experimental details are summarized in Table 1. Figure 1 shows the measured data as well as the results of the TOPAS Rietveld analysis. The quantitative results compare well to the outcomes of the VDZ Round Robin (Figure 2). There is an excellent agreement of ±1 wt. % for the main phases, with respect to the mean values of all participants. To conclude, our cost-effective desktop XRD system D2 PHASER, equipped with the 1-dimensional LYNXEYE detector, provides high quality data, which allows doing reliable quantitative phase analysis of Portland Cement Clinkers and related applications. |
Mean values and standard deviation are given in wt.%.
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D2 PHASER Desktop XRD |
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LYNXEYE 1-dimensional detector |
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Holder for automated sample preparation. |
The D2 PHASER is a portable desktop XRD instrument for research and quality control. It is easy to operate and independent of external media such as cooling circuits. Thanks to the LYNXEYE detector it is the fastest desktop XRD system on the market. The system delivers high quality measurement data, which allows performing advanced analytical methods, such as the standardless quantitative Rietveld phase analysis. This report demonstrates its use for the determination of the different sulphate phases in natural Gypsum or Anhydrite. X-ray powder diffraction combined with TOPAS Rietveld analysis is nowadays one of the most powerful methods existing, to perform quantitative phase analysis. In the last years it became a standard tool in research and development, but also in the minerals and mining industries.
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Natural Gypsum is often a mixture of the sulfate phases Gypsum (CaSO4×2H2O), Hemi-hydrate (CaSO4×½H2O) and Anhydrite (CaSO4). These phases do have different physical properties, e.g. solubility. Elemental analysis is not able to distinguish these minerals, therefore often DSC/TG methods are used. They require calibration efforts and are time consuming. XRD offers a simple and straightforward solution. A Gypsum sample of natural origin was analyzed, to demonstrate the performance of the D2 PHASER for such applications. The measurement covered the angular range from 8 to 65° 2Theta. The scan time was about 26 minutes. Experimental details are summarized in Table 1. Figure 1 shows the measured data as well as the results of the TOPAS Rietveld analysis. To conclude, our cost-effective desktop XRD system D2 PHASER, equipped with the 1-dimensional LYNXEYE detector, provides high quality data, which allows doing accurate quantitative phase analysis of the sulphate phases Gypsum, Hemi-hydrate and Anhydrite in natural rocks and flue gas purification products. |
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D2 PHASER Desktop XRD |
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LYNXEYE 1-dimensional detector |
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Holders with various cavities |
The D2 PHASER is a portable desktop XRD instrument for research and quality control. It is easy to operate and independent of external media such as cooling circuits. Thanks to the LYNXEYE detector it is the fastest desktop XRD system on the market. This report demonstrates its use for fast and reliable SAXS measurements of material exhibiting large d-spacings up to about 10 nm. Catalysts are indispensable to modern-day society because of their prominent role in petroleum refining, bulk and fine chemical processing and reduction of environmental pollution. High surface-to-volume ratios are often important for these particles since catalytic processes take place at the surface. Therefore, supports such as silica and gamma-alumina are generally used to obtain small and thermally stable particles. Fundamental studies are often hampered by the heterogeneity of conventional supports that make it difficult to disentangle the effects of the individual preparation steps on the final dispersion. To overcome these problems meso-porous silica SBA-15 (Santa Barbara no. 15) can be used as a support system. Figure 1 (left) shows the structure, which essentially consists of an amorphous silica framework forming a two-dimensional hexagonal primitive assembly of straight channels or pores. |
The structure itself is flexible and may adopt different pore diameters. The pore size can be measured from TEM pictures as shown in Figure 1 (right). X-rays play an important role in the characterization of these materials. Figure 2 shows small-angle powder data of CuO loaded SBA-15. The three peaks labeled in graph 2 are caused by the regular array of the pores. They are a measure of the average pore distance. A major advantage of powder X-ray scattering over other methods is the negligible effort needed to prepare the sample. The measurement is very fast and takes a few minutes only. Moreover, XRD has a superior sensitivity to dimensional changes of material on the below 10 nm length scale. The example presented in Figure 3 indicates that impregnation of SBA-15 with CuO during the preparation of the catalyst does not affect the long-range order of the pores in the support material. Sample and graphics are courtesy of the Inorganic Chemistry and Catalysis group, Department of Chemistry, Utrecht University, The Netherlands. |
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D2 PHASER Desktop XRD |
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LYNXEYE 1-dimensional detector |
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Holders with various cavities |
The Ratio Method implemented in DIFFRAC.DQUANT and precise intensities measured with the D2 PHASER benchtop diffractometer allow the accurate determination of retained austenite levels in steel. This helps in optimizing heat treatment which is key for tuning the mechanical properties of the steel. Quantitative phase analysis by X-ray diffraction is one of the most accurate and established methods for the determination of the amount of austenite in steel. Austenite (or gamma-iron) is a high-temperature form of iron. Upon quenching it incompletely transforms to martensite (alpha-iron, or ferrite) during the production of carbon steels. This transformation process is crucial for the strength and other mechanical properties of steel. Subsequent heat treatment during steel production may further change the austenite concentration. Furthermore the cooling conditions influence the microstructure of the steel. This is resembled in the degree of texture (or preferred orientation) of the austenite/martensite crystallites. XRD data were collected using a D2 PHASER benchtop diffractometer, equipped with a LYNXEYE linear detector and cobalt radiation. The size and shape of the samples is limited for the D2 PHASER, whereas the D8 series of instruments allows for much more flexibility in sample dimensions and geometry. |
The Ratio Method is used for calculating concentrations directly from the ratio of intensities of phases without the need for calibration. Protocols such as ASTM E 975 or SAE SP-453 provide standardized procedures for obtaining results with an accuracy level of 0.5% or better. The intensity of an X-ray powder diffraction peak is, amongst others, directly proportional to the concentration of the phase, and trigonometric intensity factors. Those factors are constant for a given experimental setup (geometry and wavelength), diffraction peak and crystal structure. The trigonometric factors can be taken from literature, or can be directly calculated from available crystallographic data. Using the respective trigonometric factors, the ratios of the intensities therefore directly yield the concentrations. Figure 1 shows the graphical definition of the peak ranges for the intensity determination. From these intensities and the respective trigonometric factors ratios are defined in the expression editor (see Figure 2). Those ratios correspond to the concentration of retained austenite in the martensite matrix. In the method, multiple pairs of peaks are used. If differences in concentration calculated from different pairs are observed, this is indicative of texture in the material. |
X-ray diffraction (XRD) is an essential technique in the analysis of shale rock formations, allowing for qualitative and quantitative mineralogical characterization. This information provides insight into wellsite behavior and enables better steering decisions, tailoring of drilling fluids, calculations of brittleness and hardness, understanding of chemical reactivity, and more. In this lab report, we discuss the mineralogical analysis of drill cuttings from shale rock using the D2 PHASER mobile X-ray diffractometer. Introduction The analysis of shale reactivity typically involves a variety of analytical techniques, including but not limited to X-ray diffraction, X-ray fluorescence, gamma logging, optical microscopy, electron microscopy, total organic content, and cation exchange capacity. From a mineralogical perspective, XRD is widely considered to be the favored technique, particularly for discrimination between elementally similar phases. For example, hematite (Fe2O3) and siderite (FeCO3) give similar elemental signatures but distinct diffraction patterns. Diffraction data are often obtained for both vertical and horizontal segments of wellbores. Analysis of the vertical section allows for the identification of zones with desirable physical properties. In horizontal segments of unconventional reservoirs, XRD is primarily used in geosteering, to ensure that the wellbore stays within a specific geological bed. Although the exact mineralogical composition changes from site to site, the more frequently observed rocks include clastics, carbonates, and clays. A more detailed list of commonly occurring minerals is given in Table 1. Wellsite geologists employ a number of different models and equations to calculate rock properties. For example, a higher value for Young’s modulus indicates a stiffer rock that is easier to fracture. Similarly, Poisson’s ratio can be used to determine rock strength. Quantitative mineralogy, including calculations of total quartz and carbonate content, can be used to provide additional information, such as brittleness indices for determining the brittleness within a specific region of a reservoir.[1, 2] Generally speaking, higher quartz and carbonate concentrations are associated with more brittle rocks and higher clay concentrations indicate a more elastic (i.e., more difficult to fracture) region. Core segments, particularly full diameter cores, are the ideal sample for thorough analysis, but are typically not used for mineralogical analysis due to practical or economic considerations. However, drill cuttings (Figure 2) are readily available at the wellsite and share the same mineralogical properties as the core. This allows XRD analysis of the cuttings to be conducted onsite and, when sampled at regular intervals, provide a useful picture of the mineralogy as a function of measured depth, leaving more of the core segments available for techniques such as fracture development tests. In this report, we present powder X-ray diffraction results of shale cuttings from a lateral well segment using the D2 PHASER (Figure 1) mobile benchtop diffractometer. |
Experimental Drill cuttings were collected every 10 m for 170 m along a horizontal well segment. The collected drill cuttings were rinsed with dichloromethane to remove residual oil and organic matter and then dried for several days in an oven. The clean cuttings were then ground to a fine particle size using a micronizing mill. Diffraction specimens were prepared by using back-loaded sample holders to reduce the effects of preferred orientation. Materials were analyzed using a D2 PHASER with cobalt (Co) radiation and a high speed silicon strip detector (LYNXEYE). Total scan time was approximately fifteen minutes per sample. Diffraction data were analyzed using two software programs: DIFFRAC.EVA for identification of mineralogical phases and DIFFRAC.TOPAS for quantification. Discussion For qualitative analysis, XRD can be used as a fingerprinting tool to identify crystalline phases based on characteristic peak locations and intensities. Representative data from a shale sample is shown in Figure 3. Major phases include quartz, calcite, dolomite, and several clay species. Reference patterns from the ICDD PDF-4 database are provided along the 2-Theta axis for reference. It is important to note the exceptional data quality – with respect to peak resolution, signal-to-noise, and instrument background – across the entire scanning range. Narrow peak resolution is important for resolving closely spaced reflections, which are commonly observed in complex mixtures like naturally occurring rocks. Low achievable background, when combined with the reflection geometry of the D2 PHASER, allows for accurate measurement of low angle peaks and speciation of clay minerals. A waterfall plot of all collected data is shown in Figure 4, highlighting the similarities in diffraction patterns. This indicates comparable mineralogical compositions and – as these samples were obtained from a lateral segment – good geosteering. Weight percentages of each observed phase were calculated using quantitative Rietveld analysis with DIFFRAC.TOPAS. A standardless quantification model was used for these samples, which eliminates the need for separate calibration curves with pure standards. Rietveld analysis also allows for more robust quantification due to the ability to account for preferred orientation, absorption effects, peak overlap, and varying cationic occupancies (e.g., different compositions within potassium-rich feldspars). Data for a representative sample is shown in Figure 5. The same refinement model was applied to each data set and quantification is shown in Figure 6. Carbonate minerals and feldspars are combined into two separate groups for clarity and easy of viewing. Clay minerals include both swelling and non-swelling members as well as chlorites, which are occasionally left as a distinct group. Although decisions vary from site to site, optimal shale compositions generally have a combined weight percent of > 50-60% for quartz, feldspars, and carbonates.[3] |
Phase | Minerals | Chemical Formula |
Silica | Quartz Cristobalite |
SiO2 SiO2 |
Feldspars | Albite Orthoclase Anorthite Plagioclase |
NaAlSi3O8 KAlSi3O8 CaAl2Si2O8 NaAlSi3O8 - CaAl2Si2O8 |
Carbonates | Calcite Dolomite Siderite Ankerite |
CaCO3 CaMg(CO3)2 FeCO3 Ca(Fe,Mg)(CO3)2 |
Clays | Illite Montmorillonite Chlorite Muscovite Kaolinite |
Kx(Al,Mg)2(Si,Al)4O10(OH)2 (Na,Ca)0.33(Al,Mg)2Si4O10(OH)2 (Mg,Fe)5Al(Si,Al)4O10(OH)8 KAl2(AlSi3O10)(OH)2 Al2Si2O5(OH)4 |
Additional Phases | Pyrite Gypsum Apatite Hematite |
FeS2 CaSO4∙2H2O Ca5(PO4)3F Fe2O3 |
Note that given chemical formulae are representative. Exact compositions - especially for feldspars and clays/phyllosilicates - will vary due to intercalations and ionic substitutions.
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D2 PHASER Desktop XRD |
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Holders with various cavities |
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LYNXEYE 1-demensional detector |
The D2 PHASER is a mobile benchtop X-ray diffractometer (XRD) used in the identification of both bulk and clay minerals within geological samples. In this report, we describe the analysis of clay samples using oriented mounts. Diffraction studies enable the differentiation between swelling and non-swelling clays by observing the shifting of diffraction peaks due to expansion in swelling clays. Introduction Clay minerals comprise a large class of fine-grained, layered silicates that result from the weathering of bulk minerals. Clays are of particular interest for the mining and drilling industries due to the physical properties they impart on surrounding geological formations. Here, we discuss the qualitative analysis of clays by X-ray diffraction (XRD) with the D2 PHASER benchtop diffractometer (Figure 1), specifically towards identifying swelling clay species. Although there are quite a number of discrete clay species and interstratifications, clay minerals can be roughly arranged into three major groups: kaolinite, illite, and smectite. Vermiculites are often considered as a fourth classification. Other phyllosilicate minerals of interest include micas and chlorites, which are sometimes included in the analysis of clay minerals, though neither are explicitly clays. Of the three major groups, smectites are distinguished by the ability to absorb moisture and the concomitant demonstration of volumetric expansion. As such, members of the smectite group, like montmorillonite, are often referred to as swelling clays. As mentioned previously, clay minerals are a key concern in many drilling applications. For example, in the hydraulic fracturing industry, high concentrations of clays indicate higher ductility and can lead to poor fracture formation. Additionally, the presence of swelling clays can lead to water-induced swelling during the initiation process or negative effects, such as self-healing, during production stages. The identification of these minerals is essential for developing tailored solutions for additives and stabilizers. In this report, we demonstrate the identification of swelling clays using a mobile, benchtop diffractometer and a few simple pieces of laboratory equipment. Overview and Experimental Samples were prepared as air-dried and glycolated oriented mounts according to the procedure outlined by the U. S. Geological Survey (USGS).[1] The oriented mount causes the plate-shaped clay mineral particles to lie flat along the substrate surface allowing the basal diffraction peaks to be probed using XRD symmetric scans in reflection geometry. The basal plane spacing (or d-spacing) can be calculated by determining the diffraction peak angle (in degrees 2Theta) of a diffractogram. The initial d-spacing and the degree of expansion or contraction, after certain treatments such as glycolation, allows the identification of clay minerals including swelling clays. For example, the addition of glycol to smectite clays results in expansion of the basal planes as polyol molecules intercalate between atomic layers, forcing them apart. The associated reflection in diffraction data will shift to a larger d-spacing and smaller diffraction angle as predicted by Bragg’s Law. Non-swelling clays will not demonstrate this lattice expansion. As such, the associated diffraction peaks will remain in the same location both before and after glycolation. |
A bulk sample of shale rock was ground using a micronizing mill and dispersed in water via sonication (Figure 2). A small amount of sodium hexametaphosphate, a dispersant, was added to aid in breaking up flocculated clay particles and agglomerates. Bulk minerals were allowed to settle for one hour prior to collecting the clay minerals (Figure 2). The supernatant with the clay fraction was separated by decanting and set aside for the preparation of oriented mounts. Although this can be done gravimetrically, the use of a centrifuge can rapidly speed up the process. Oriented mounts were prepared by depositing the dispersed clay particles onto glass slides and allowing the suspension to dry. Additional sample was added dropwise until an opaque film was acquired. The dried oriented mounts were analyzed via XRD and then modified by glycolation. This was done by carefully applying a small drop of ethylene glycol to the surface of the clay and allowing it to absorb (Figure 3). Multiple clay mounts can be batch-processed by placing in a warm desiccator filled with a small amount of ethylene glycol for several hours. A second diffraction scan was collected after treatment for comparison to the original oriented mount. Additional mounts were prepared from several commercially available clay standards for demonstration purposes. Data was collected in reflection geometry using D2 PHASER equipped with a high-speed linear detector (LYNXEYE), which is essential for rapid data collection. The D2 PHASER is capable of being operated in a mobile lab environment, featuring an on-board cooling system, integrated computer, and operating with standard domestic power. The scanning range should start at ≤ 3 ° 2θ in order to ensure that the clay peaks of interest are fully and properly. Total data collection time for these two scans is 10 minutes. Total processing time for each sample is about 3 hours, mostly unattended during separation and drying steps. Discussion Two scans were collected on each prepared sample. The first scan was collected on the untreated oriented slide. The second scan was collected on the fully swelled and glycolated slide. Low angle diffraction data for two clay samples is shown in Figure 4. A dramatic shift to a larger d-spacing is observed for the bentonite sample, indicating sample swelling. The kaolinite reflections are unaffected. For the collected clay fraction, several mineral species were observed, as shown in Figure 5, including strong reflections from chlorite and muscovite. Although the smectite reflection is severely broadened in the oriented mount – to the point [1] Poppe, L.J.; Paskevich, V.F.; Hathaway, J.C.; and Blackwood, D.S., A Laboratory Manual for X-Ray Powder Diffraction; U.S. Geological Survey Open-File Report 01-041; Woods Hole, MA, 2001. |
Diffraction data for two clay samples – bentonite and kaolinite – as both oriented mounts and glycolated specimens. The clear shift in low angle data for the bentonite sample indicates expansion along the c-axis. The kaolinite sample does not swell with the addition of glycol; consequently, the reflection is observed at the same location.
Diffraction data for a clay fraction collected from shale rock. Chlorite and muscovite reflections are easily detected and do not shift upon glycolation. The broad smectite reflection is difficult to observe in the oriented mount but appears as a stronger, shifted reflection after the addition of ethylene glycol.
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D2 PHASER Desktop XRD |
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Holders with various cavities |
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LYNXEYE 1-demensional detector |
Our D2 PHASER delivers uncompromisingly good and reliable analyses. The strict quality standards of our entire product range are applied to the assembling, testing and certified safety of the D2 PHASER! We give you our word: Good Diffraction Practice and Best Data Guarantee! Safety assurance: Each instrument always complies with the world’s highest statutory requirements regarding X-ray safety, machine and electrical safety. This certainty is obtained after stringent scrutiny by independent institutions. Two independent, fail-safe safety circuits and “X-ray On” monitors guarantee that the most recent radiation and personal safety regulations are observed. The D2 PHASER is pre-aligned at delivery. Every single instrument must pass our strict test procedure, which is based on the internationally accepted reference material corundum. The corundum reference is supplied with the instrument, so you can check your instrument at any time. Detector guarantee: We guarantee that our 1-dimensional LYNXEYE is absolutely faultless! This is due to Bruker AXS’ unique detector design. By integrating the LYNXEYE detector in the D2 PHASER it becomes the fastest and most efficient desktop diffractometer in the world. The best in its class: the D2 PHASER. |
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X-ray analysis has never been easier! This is how X-ray analysis works: It goes without saying that the software solutions of our DIFFRAC.SUITE go beyond this. In the DIFFRAC.SUITE the full scope of functions is available. Using the COMMANDER, CONFIGURATION and TOOLS plug-in the expert has control over administration of experiment databases, user rights and all the way through to 21 CFR Part 11. Everything on the system works in a safe, simple and reliable way. DIFFRAC.SUITE - performance made-to-measure: easy for anyone to operate, full functionality and control for experts. Integrated within a networked world. The D2 PHASER is a full-blown diffractometer: its measured data is fully compatible with all of our DIFFRAC.SUITE solutions. The familiar world of search/match and structure databases, EVA, TOPAS, DQUANT ,… all of this is available to the XRD specialist for identifying, quantifying and determining the characteristics of the crystalline phases. D2 PHASER – Welcome to the world of Bruker AXS! |
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D2 PHASER: Technical Data
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Geometry | Theta / Theta |
Max. useable angular range (depending on detector) |
–3 … 151.4 ° 2Theta |
Accuracy | ± 0.02° throughout the entire measuring range |
Achievable peak width | < 0.04° |
Alignment | Not needed, factory aligned |
X-ray wavelengths | Cr / Co / Cu, standard ceramic sealed tube |
X-ray generation | 30 kV / 10 mA |
Detectors | 1 dimensional SSD160-2, 1 dimensional LYNXEYE-2, 1 dimensional LYNXEYE XE-T |
Stages | Single position, Ø 51 mm, programmable sample rotation Motorized 6 position, Ø 32 mm programmable sample rotation |
Sample holders |
Various cavities, low background with and without cavity, air-tight, sealed, filter samples,back loading, oriented slides (clay) |
Instrument type | Portable, benchtop |
Exterior Dimension | 61 x 60 x 70 cm (h x d x w) 24.02” x 23.62” x 27.56” |
Weight | 95 kg |
Power supply | 90 – 250 V |
External cooling water supply | None |
Computer | Built-in Optional additional PC connected via LAN interface |
Interfaces | 2 x USB and 1 x LAN |
D2 PHASER™, US 7,852,983 B2, EP2 112 505 B1, DE 102 008 020 108 B3 patent. LYNXEYE™ EP 1 510 811 B1 patent. DIFFRAC is a registered trademark of the US Office of Patents and Trademarks. Goniometer EP 2 112 505 A1. |
Need more information?
Our team is happy to assist and answer your questions.
Please send an e-mail to: info.baxs@bruker.com.