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D2 PHASER 2nd Generation

Take a look under the hood of the world fastest X-ray benchtop diffractometer.

Latest Lab Report

New application report

Application Report 85: Powder X-ray diffraction (XRD) of swelling clays

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Contact us for more information on the 2nd generation of the D2 PHASER

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D2 PHASER 2nd Gen with opened front cover

USB and Ethernet connectors

Internal chiller

1-dimensional LYNXEYE detector

Transport handles

Status display LEDs

All-in-one analysis

Simple sample loading

     

D2 PHASER – The Second Generation Benchtop X-Ray Diffractometer

  • Compact all-in-one desktop design
  • Innovative high-end goniometer design
  • Integrated PC / monitor
  • DIFFRAC.SUITE software
  • Leading detector technology
  • D2 PHASER – all-in-one desktop design

The new D2 PHASER is the next generation benchtop diffractometer for all X-ray powder diffraction applications. The new D2 PHASER is equipped with an integrated PC and a flat screen monitor. The new version of the DIFFRAC.SUITE software allows measurement and analysis right out of the box. Equipped with a LYNXEYETM compound silicon strip detector, the D2 PHASER is able to collect high quality data with unprecedented speed. The new sample changer allows to run batches of up to 6 samples.

We implemented innovative technologies to make the D2 PHASER the most compact and fastest, all-in-one phase analyzer available on the market. The unit is mobile and easy to install with only the need for standard electrical power. It is therefore ideal for laboratory or on-location operation, in other words, it is a true Plug’n Analyze system.

Ease-of-use, high performance and low cost of ownership are the key features of the D2 PHASER. The diffractometer was developed to open new applications and markets beyond traditional XRD analysis. D2 PHASER – the price/ performance leader for XRPD in laboratories and QC/PC applications for e.g. cement, industrial minerals, geology, chemistry, pharmaceuticals, as well as for educational.

Main features

Plug’n Analyze

  • A simple domestic wall socket is all you need

  • No installation

  • No alignment
  • No instrument configuration

  • No infrastructure

  • No pre-installation requirements

All-in-one analytics

  • Simple sample loading

  • Industrial standard sample holders

  • Theta/Theta geometry, horizontal samples
  • Fully-fledged integrated PC

  • On-site and remote operation

LYNXEYE detector

  • Intensity increases by a factor of more than 150

  • 100% working strips at delivery – guaranteed

  • Energy discrimination for sample fluorescence suppression
  • 1-D scanning and snapshot mode; 0-D mode

  • Angular coverage > 5.5° 2Theta

X-ray source

  • Common sealed X-ray tube design

  • Low power load – no tube ageing
  • Virtually infinite tube lifetime

  • Cr, Co, Cu radiation

Desktop design

  • Minimum space requirements

  • Handles for convenient transportation

  • Maximum X-ray safety with radiation level significantly below 1μSv/h
  • Clearly visible warning and operating elements

  • Angular accuracy better than ±0.02° 2Theta – guaranteed

Island-mode

  • Internal cooling system
  • Stand-alone operation built in computer

Automatic sample changer

  • 6 sample positions

  • 32 mm sample holder diameter
  • user defined rotation speed

D2 PHASER – the desktop giant

  • Phase identification and quantification
  • Degree of crystallinity determination
  • Phase properties (cell parameters, crystallite size, and lattice strain)
  • Crystal structure analysis
  • Wide variety of different sample holders of industrial standard dimension (Ø 51.5 mm)

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 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.

With a performance enhancement in terms of intensity by a factor of more than 150, the D2 PHASER is actually playing in the top class. Additionally the LYNXEYE allows suppression of sample fluorescence providing an excellent peak-to-background ratio even for strongly fluorescent samples, eliminating any need for secondary monochromators.

D2 PHASER – X-ray diffraction in a new dimension!

Holders

Holders with various cavities
Holder for automated sample preparation.
Holder for clays
Low back ground holder for small sample amounts
Airtight holders for environment sensitive samples
Holder for filter samples

All-in-one is everything you need – D2 PHASER

  • Minimal electrical power consumption (650 W)
  • No cooling water supply
  • No significant tube ageing – practically endless tube lifetime
  • Minimal space required

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!

D2 PHASER – X-ray diffraction tool for everyone – everywhere!

Get more information on www.bruker.com.

Industries

Cement & Raw Materials
Minerals & Mining
Geology & Exploration
Ceramics
Chemistry & Catalysts
Research & Education
Pharmaceuticals
Environment

D2 PHASER Desktop XRD:
Phase Identification of Geological Material

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.

Figure 1: Phase identification of geological material with DIFFRAC.EVA

The major phase is gypsum. Semi-quantitative phase analysis gives the content of the minor phases: quartz (7.2%), muscovite (0.9%), dolomite (2.1%), and chlorite (1.0%).

Table 1: Experimental settings

  • Cu radiation (30 kV, 10 mA), Ni filter

  • Continuous scan from 0.6 to 10.0° 2Theta, Step width 0.01° Counting time 0.2 sec per step

  • Total scan time about 4 min.

  • 2.5° Soller collimators, 0.1 mm divergence slit, secondary anti-scatter slit 3mm, air-scatter screen over sample closed to 0.1 - 0.2 mm

  • LYNXEYE detector opening 1° 2Theta
D2 PHASER Desktop XRD
Holders with various cavities
LYNXEYE 1-dimensional detector

D2 PHASER Desktop XRD:
Anode Coke (Lc Value) Analysis

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.

Figure 1: Determination of the full width of petroleum coke using DIFFRAC.EVA

Determination of the full width at half maximum of the 002 peak of petroleum coke using DIFFRAC.EVA. The software evaluates the peak shape and automatically calculates the crystallites size (36.5 Å) using the Scherrer equation.

Table 1: Experimental settings

  • Cu radiation (30 kV, 10 mA), Ni filter

  • Continuous scan from 14.0 to 38.0° 2Theta, Step width 0.2°, counting time 0.1 sec per step

  • Total scan time about 30 sec.

  • 2.5° Soller collimators, 1.0 mm divergence slit, anti-scatter screen

  • LYNXEYE detector opening 5° 2Theta
D2 PHASER Desktop XRD
LYNXEYE 1-dimensional detector
Holders with various cavities

D2 PHASER Desktop XRD:
Silica Dust Analysis

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.

Figure 1: DIFFRAC.EVA

No Titel

 

Diffraction signals of a blank, 12, 30, 90, 150, and 210 µg quartz on filters at the position of the strongest quartz peak all measured with 1 sec per step. The inset shows the calibration curve of the net intensities determined using DIFFRAC.EVA vs. the known concentrations.

Table 1: Experimental settings

  • Cu radiation (30 kV, 10 mA), Ni filter

  • Continuous scan from 26.1 to 27.1° 2Theta, Step width 0.01°
    Counting time:
    1) > 30 μg: 1 sec per step
    2) < 30 μg: 5 sec per step
    1) Total scan time 5 min.
    2) Total scan time 25 min.

  • 4° Soller collimators, 1.0 mm divergence slit, anti-scatter screen

  • LYNXEYE detector opening 5° 2Theta
D2 PHASER Desktop XRD
LYNXEYE 1-dimensional detector
Holder for filter samples

D2 PHASER Desktop XRD:
Crystal Structure of Er-Melilite

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:
[1] Peters, L., Knorr, K. & Depmeier, W.: Z. Anorg. Allg. Chem. 2006, 632, 301-6

Figure 1: TOPAS plot of x=0.5 Er-melilite

Lattice parameters of the tetragonal unit cell are a=7.6931(9) Å and c=5.0550(6) Å. The refined fractional coordinates are plotted in the inset vs. literature data [1]. Agreement parameters of the TOPAS refinement are Rwp=3.14, Rp=2.38, and GoF=2.02.

Table 1: Experimental settings

  • Cu radiation (30 kV, 10 mA), Ni filter

  • Continuous scan from 10 to 100° 2Theta, Step width 0.02°, Total counting time 2.5 sec per step

  • Total scan time about 80 min.

  • 2.5° Soller collimators, 0.6 mm divergence slit, anti-scatter screen

  • LYNXEYE detector opening 5° 2Theta

 

D2 PHASER Desktop XRD
LYNXEYE 1-dimensional detector
Low back ground holder for small sample amounts

D2 PHASER Desktop XRD:
Quantitative phase analysis of OPC Clinkers

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.

Figure 1: TOPAS Rietveld phase quantification of the VDZ Round Robin Clinker sample

TOPAS Rietveld phase quantification of the VDZ Round Robin Clinker sample (values given in wt. %). The blue curve is the measured diagram. The red curve is the calculated diagram. In grey the difference of both is given. The marks below indicate the possible peak positions of each phase.

Figure 2: Outcomes of the VDZ Round Robin 2005

Mean values and standard deviation are given in wt.%.

Table 1: Experimental settings

  • Cu radiation (30 kV, 10 mA), Ni filter
  • Continuous scan from 0.6 to 10.0° 2Theta, Step width 0.01° Counting time 0.2 sec per step
  • Total scan time about 4 min.
  • 2.5° Soller collimators, 0.1 mm divergence slit, secondary anti-scatter slit 3mm, air-scatter screen over sample closed to 0.1 - 0.2 mm
  • LYNXEYE detector opening 1° 2Theta
D2 PHASER Desktop XRD
LYNXEYE 1-dimensional detector
Holder for automated sample preparation.

D2 PHASER Desktop XRD:
Quantitative phase analysis of Gypsum/Anhydrite 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. 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.

 

 

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.

Figure 1: TOPAS Rietveld phase quantification of the Gypsum sample

TOPAS Rietveld phase quantification of the Gypsum sample (values given in wt. %). The blue curve is the measured diagram. The red curve is the calculated diagram. In grey the difference of both is given. The marks below indicate the possible peak positions of each phase.

Table 1: Experimental settings

  • Cu radiation (30 kV, 10 mA), Ni filter
  • Continuous scan from 0.6 to 10.0° 2Theta, Step width 0.01° Counting time 0.2 sec per step
  • Total scan time about 4 min.
  • 2.5° Soller collimators, 0.1 mm divergence slit, secondary anti-scatter slit 3mm, air-scatter screen over sample closed to 0.1 - 0.2 mm
  • LYNXEYE detector opening 1° 2Theta
D2 PHASER Desktop XRD
LYNXEYE 1-dimensional detector
Holders with various cavities

D2 PHASER Desktop XRD:
SAXS-Analysis of the Mesoscopic Catalyst SBA-15

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.

Figure 1: Schematic view of zeolite SBA-15

Schematic view of zeolite SBA-15 (left). This material exhibits pores up to 10 nm diameter which is larger than for other meso-porous materials such as MCM-41. The size of the pores is also seen on TEM picture (right).

Figure 2: Small-angle X-ray powder pattern of CuO loaded SBA-15

Small-angle X-ray powder pattern of CuO loaded SBA-15. The three signals correspond to the 100, 110 and 200 reflections on a hexagonal primitive lattice. They are used to estimate the average pore distance of this material, here about 11.25 nm.

Table 1: Experimental settings

  • Cu radiation (30 kV, 10 mA), Ni filter
  • Continuous scan from 0.6 to 10.0° 2Theta, Step width 0.01° Counting time 0.2 sec per step
  • Total scan time about 4 min. LYNXEYE 1-dimensional detector
  • 2.5° Soller collimators, 0.1 mm divergence slit, secondary anti-scatter slit 3mm, air-scatter screen over sample closed to 0.1 - 0.2 mm
  • LYNXEYE detector opening 1° 2Theta
D2 PHASER Desktop XRD
LYNXEYE 1-dimensional detector
Holders with various cavities

DIFFRAC.DQUANT:
Norm compliant quantification of retained austenite

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.

Figure 1: Standard scan chart in DIFFRAC.DQUANT

Standard scan chart in DIFFRAC.DQUANT. The orange and green colors represent the integration ranges for austenite and martensite, light blue ranges correspond to background areas.

Figure 2: Concentration/Intensity chart in DIFFRAC.DQUANT

Concentration/Intensity chart in DIFFRAC.DQUANT. The lower panel represents the background corrected integral intensities as defined graphically (see Figure 1). The upper panel shows the austenite concentrations expressed as intensity-ratio modules, which are defined in the expression editor.

X-Ray Diffraction in the Petrochemical Industry:
Wellsite Mineralogical Analysis of Shale Formations with the D2 PHASER

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]

References

[1] Jarvie, D. M.; Hill, R. J.; Ruble, T. E.; and Pollastro, R. M. AAPG Bulletin 2007, 91, 475.
[2] Wang, F. P. and Gale, J. F. W. GCAGS Transactions 2009, 59, 779.
[3] Scotchman, I. C. Exploration for Unconventional Hydrocarbons: Shale Gas and Shale Oil. In Fracking: Issues in Environmental Science and Technology; Hester, R. E. and Harrison, R. M., Eds.; The Royal Society of Chemistry: Cambridge, UK, 2015; pp 84-86.

Table 1: Some commonly occuring minerals in shale formations

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.

Figure 1: D2 PHASER benchtop diffractometer with LYNXEYE detector

D2 PHASER benchtop diffractometer with LYNXEYE detector.

Figure 2: Core segments and drill cuttings

Core segments and drill cuttings

Figure 3: Representative diffraction data from a shale sample

Representative diffraction data from a shale sample. Mineralogical phases were identified with DIFFRAC.EVA. Database patterns for identified phases are provided along the 2-Theta axis for reference.

Figure 4: Waterfall plot for all samples

Waterfall plot for all samples. A y-offset was applied for ease of viewing and to illustrate the similarities in diffraction data.

Figure 5: Quantitative Rietveld refinement with DIFFRAC.TOPAS

Quantitative Rietveld refinement with DIFFRAC.TOPAS. Collected data is plotted in blue. Refined data is plotted in red. A difference curve between collected and refined data is plotted in grey.

Figure 6: Overall mineralogy plotted as a function of measured depth

Overall mineralogy plotted as a function of measured depth. Brittle rocks generally contain high concentrations of quartz, carbonates, and feldspars and low concentrations of clay minerals.

D2 PHASER Desktop XRD
Holders with various cavities
LYNXEYE 1-demensional detector

X-Ray Diffraction in the Petrochemical Industry:
Identification of Swelling Clays with the D2 PHASER

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
of being difficult to confirm visually – the swelled mount displays a very clear shifted reflection centered around 17.4 Å, confirming the presence of swelling clays in this sample.

References:
[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.

Figure 1: D2 PHASER benchtop diffractometer

D2 PHASER benchtop diffractometer.

Figure 2: Ground geological samples

Finely ground geological samples are dispersed in water via sonication (left). The bulk and clay mineral fractions are divided by gravimetric separation (right), and the clay minerals are collected by decanting. The markings on the beaker are for tracking the progress of separations.

Figure 3: Prepared clay slides

Prepared clay slides are placed in a sample holder with adjustable height (top) for accurate positioning within the diffractometer. Clay specimens are analyzed as a dry oriented mount (bottom left) and again following the addition of ethylene glycol (bottom right).

Figure 4: Diffraction data for two clay samples

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.

Figure 5: Diffraction data for a clay fraction collected from shale rock

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.

D2 PHASER Desktop XRD
Holders with various cavities
LYNXEYE 1-demensional detector

D2 PHASER – dataquality, functionality
and safety without any compromises

 

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.

Alignment guarantee:

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. Shake on it!

Advanced features

XRD on polycrystalline material –more intensity with LYNXEYE detector

  • In an XRD experiment performed on polycrystalline material the incident X-ray beam is diffracted by innumerous crystallites in specific 2Theta directions.

    To record the exact 2Theta positions a narrow slit in front of a point detector is required.
  • The LYNXEYE literally provides more than 150 integrated slits, allowing more than 150 2Theta positions to be recorded simultaneously

Instrument alignment – a sound base for accuracy!

  • Angular accuracy ≤ ± 0.02° 2Theta over the whole angular range – guaranteed!
  • Why is this important? Accurate and verifiable instrument alignment is a basic requirement for accurate and reliable phase identification or structure analysis.

Unrivaled resolution

  • Very small peak width of less than 0.05° 2Theta obtained by high-resolution XRD measurement of LaB6 (NIST SRM 660a) with LYNXEYE detector; 0.1° divergence and 1.5° Soller slit.
  • Why is this important? Good instrument resolution is a prerequisite to resolve overlapping diffraction peaks in complex powder patterns.

The ultimate in ease of use –
D2 PHASER with DIFFRAC.SUITE

  • Compatible with the entire Bruker AXS’ Diffraction Solutions family
  • Fully network capable
  • Support of different user levels and modes
  • EVA – powerful phase identification
  • TOPAS – sophisticated quantitative phase and structure analysis

X-ray analysis has never been easier! Even inexperienced users produce perfect measurements from the very beginning thanks to the DIFFRAC.SUITE Easy-mode.

This is how X-ray analysis works in the Easy-mode:

Select COMMANDER plug-in, enter measurement time and angular range and start. That’s all!

If a method has already been defined, it goes even faster:

Select START JOBS, click on Method and off you go!

It goes without saying that the software solutions of our DIFFRAC.SUITE go beyond this. In Expert-mode the full scope of functions is available. Using the COMMANDER, CONFIGURATION and TOOLS plug-in the expert has control over administration of experimental databases, user rights and all the way through to the Audit Trail. 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.

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!

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,… 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!

DIFFRAC.SUITE

DIFFRAC.DQUANT, Quantitative Analysis

  • Quanitative analysis from calibration to reporting
  • Based on single-peak intensities
  • Interactive, batch-mode and console-mode operation
  • One software - numerous methods
    - Addition method
    - Standard-less ratio method
    - Standards based calibration methods

DIFFRAC.EVA

  • Qualitative phase identification
    - ICDD PDF2 and PDF4
    - User-defined databases
  • Semi-quantitative phase analysis
    - RIR method
    - Combined XRD-XRF analysis

  • Publication-ready reporting

DIFFRAC.TOPAS, Quantitative Analysis

  • Quantitative phase analysis
    - Crystalline phases
    - Amorphous phases

  • Degree of crystallinity determination
  • Spiking method

  • PONKCS method

DIFFRAC.TOPAS, Structure Analysis

  • Indexing (LSI and LP-Search methods)

  • Pawley and LeBail fitting

  • Rietveld structure refinement
  • Ab-initio structure determination
    - Simulated annealing
    - Charge Flipping
    - 3D Fourier analysis

  • Microstructure analysis

Easy-mode

  • (1) Real-time measurement display
  • (2) Straightforward selection of scan parameters:
    - Angular range
    - Step size
    - Measurement time

Expert-mode

  • (1) Real-time measurement display

  • (2) Straightforward selection of scan parameters:
    - Angular range
    - Step size
    - Measurement time
  • (3) Full access to all settings:
    - User management
    - Database maintenance
    - Instrument configuration
    - Service tools

  • (4) Full access to all instrument parameters:
    - Drives
    - Detector settings
    - Generator settings

X-ray on status LEDs

No Titel

D2 PHASER 2nd Gen with opened front cover

USB and Ethernet connectors

Internal chiller

1-dimensional LYNXEYE detector

Transport handles

Status display LEDs

All-in-one analysis

Simple sample loading

     

Holders with various cavities

Holder for automated sample preparation

Holder for clays

Low back ground holder for small sample amounts

Airtight holders for environment sensitive samples

Holder for filter samples

   

Cement & Raw Materials

Minerals & Mining

Geology & Exploration

Ceramics

Chemistry & Catalysts

Research & Education

Pharmaceuticals

Environment

D2 PHASER – ease of operation

     
 
D2 PHASER: Technical Data
Geometry Theta / Theta
Max. useable angular range
(depending on detector)
–3 … 160 ° 2Theta

Accuracy ± 0.02° throughout the entire measuring range
Achievable peak width < 0.05°
Alignment Not needed, factory aligned
X-ray wavelengths Cr / Co / Cu, standard ceramic sealed tube
X-ray generation 30 kV / 10 mA
Detectors Scintillation counter, 1-dimensional LYNXEYE, energy-dispersive XFlash 430
Sample stages - single sample stage for 51.5 mm Ø sample rings
- automatic 6 position sample changer for 32 mm Ø sample rings
Sample motion Spinning with user defined speed
Instrument type Mobile, 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 patent, EU patent pending;
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.

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