Analytical technologies for catalyst
manufacture and research
Understand the physical properties and chemical constitutionof your catalyst materials

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The power ofheterogeneous catalysis

State-of-the-art equipment formaterial characterization

Heterogeneous catalysts have been at the heart ofthe chemicals industry for over 100 years, enablingtransformations ranging from the production ofcommodity and fine chemicals to the removalof harmful gases from vehicle exhaust.

Carrying out precise chemical transformations mediatedby heterogeneous catalysts requires materials thatare highly complex, usually in terms of their physicalmicrostructure, and often in terms of their chemicalcomposition as well.

But now, we’re witnessing the emergence of a
new era in catalyst application, driven by thedemand to extract value from waste feedstocks,
find environmentally benign routes to transport
fuels, and use scarce elements more wisely.

Staying ahead in this race to capitalize on emerging
markets requires a better understanding of the underlying
physical and chemical properties of catalyst materials– and that’s where Malvern Panalytical can help. With
over 60 years’ experience in designing, manufacturing
and supplying analytical instruments for all types ofmaterials, we’re ready to advise you on investigating
the material properties of your heterogeneous
catalysts, whether you’re in research or production.

Wastevalorization

Commodity andfine chemicals
synthesis

Polymer
synthesis

CATALYSTS‘Green’ hydrogengeneration andfuel cells

Conventional
fuel production

Environmental
remediation

Alongside their long-established roles
in synthesis of industrial chemicals,
polymers and petrochemical-derived
fuels, catalysts are increasingly playing
a central role in the green transition
to circular industrial processes with alow environmental footprint. Malvern
Panalytical’s equipment can help you
achieve your sustainability goals by
understanding the material properties ofcatalysts in more depth than ever before.

Characterizing these materials in depth is of course
an inherent part of the research and developmentof catalysts, but it’s also valuable during catalyst
manufacture, especially for monitoring product quality andconsistency, and for troubleshooting issues arising during
production or the end application.
At Malvern Panalytical, we provide a range of instrumentsthat can help you investigate and monitor the physical,
chemical and microstructural properties of your catalystmaterials at every stage of research, development andmanufacture. These include systems for:• Stand-alone analysis – for all classes of off-line
measurement from sophisticated operando researchthrough to processing. As well as straightforward
analysis of individual samples, most systems havesample changer options that help you to create batchmeasurements and streamline your routine analyses.
• At-line analysis – for enabling robot automation ofsample handling, measurements, and analyses. Many
samples can be collected during a processing cycle
and rapidly analyzed with minimal user intervention,
freeing your analysts to deal with the troubleshooting.
• On-line analysis – for non-destructive measurementof materials during processing. These systems allow
real-time analyses of materials flowing throughproduction lines, making them ideal for quality control.
So whether you’re researching new catalysts to meet
emerging challenges, or simply ensuring that yourproducts maintain their reputation as the best in the field,
we’re in an excellent position to support you with analyticalequipment and expert advice.

45

Matching analytical solutions
to industry challenges

Developing materials withnew properties

Malvern Panalytical's products allow measurement of a variety of material properties, providing solutions for the threemain challenges faced by catalyst manufacturers and researchers.

Developing new catalysts for the rapidly changing
demands of society is a difficult balancing act, requiring
the fine-tuning of catalytic activity and/or selectivity,
alongside a deep understanding of surface properties.
This is all set against the scarcity and cost of manycatalytically active elements, and the need to improvesustainability and lessen environmental impact.

Pages 5–7 describe these three challenges in more detail, followed on pages 8–15 by details of the analytical methods,
and the equipment options available for each of them.

OPTIMIZINGAND MONITORING
MANUFACTURING
PROCESSESDEVELOPING
MATERIALS WITH
NEW PROPERTIESUNDERSTANDING
CATALYSTPERFORMANCE

Opportunities to decarbonize our economy present new
challenges. For example, electrolytic processes that
intend to use renewable sources of energy such as windand solar power must be able to cope with fluctuations
in electricity supply, which requires a fundamental
shift in catalyst design away from the steady-stateparadigm that the catalyst industry has long followed.
Fortunately, our analytical methodologies can help bothacademia and industry to resolve these challenges.

Stability
Particleshape• Reducing reliance upon scarce elements
Platinum-group elements underpin the performanceof many catalytic systems, but they are expensive,and upscaling catalytic processes is limited by theiravailability. Therefore, as well as developing new
catalysts using more readily available elements,
there is a need to minimize loadings of theseelements, by complete or partial substitution. Our
Zetium and Epsilon XRF instruments address bothchallenges, by enabling researchers to measureelemental concentrations in new catalytic materials.

PorestructurePhase
proportions

Particlesize
Image
analysis

Crystallinity
Electrophoretic
light scattering
(ELS)

X-ray
fluorescence(XRF)

Elemental
composition

X-ray
diffraction(XRD)

Crystalstructure

Impurities

E

Laser
diffraction
(LD)

-L

LI

IN

AT

Dynamic lightscattering
(DLS)

N

N

E

ST

A N D-ALO NE

O• Understanding hierarchical pore size distributions
The micro-, meso- and nano-pores often neededin catalyst materials can be highly ordered andpresent at multiple length scales, providing acomplex system of surfaces and hence a muchgreater catalytic activity than a non-porous material.
In addition to XRD structure refinement, X-ray
scattering methods such as small-angle X-ray
scattering and reflectometry are available on our
Empyrean XRD systems. Together these can probe
porosity scaling from lattice voids to nano-pores.
• Understanding local structure
The local atomic structure of catalytic materials
is central to their activity, but can change during
reaction processes. Solving the structures of strongly
crystalline materials can be carried out on our Aeris
and Empyrean XRD systems, but the Empyrean
can also be used to investigate subtle changes inamorphous or highly defective structures using total
scattering and pair distribution function analysis(PDF). This avoids the need to resort to synchrotron
sources, and so enables more flexible, timely analysis.

• Characterizing substrate particles during loading
Characterizing substrate particles before and after
loading with catalytically active material may be
useful to ensure that no undesirable changes inparticle morphology or chemistry have taken place. As
well as our Mastersizer and Insitec LD and Zetasizer
DLS instruments for characterizing particle size,
we also offer Aeris and Empyrean XRD systems, forobtaining a detailed understanding of phase changes.
• Controlling the distribution of active sites on
catalyst supports
Impregnation of active metals onto a catalyst
support is one of the major routes to heterogeneous
catalysts, but an uneven distribution of metal
nanoparticles can give rise to poor levels ofactivity. This distribution is influenced by thesurface charge of the catalyst support, making
measurement of zeta potential by ELS useful during
the development phase of catalyst research.

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Optimizing and monitoring
manufacturing processes

Understanding catalyst
performance

Good process control is central to catalyst manufacturing,and can be used to check that materials at all stagesof production meet the desired standards, and also
to optimize processes (especially on scale-up) to
reduce costs. From an analytical standpoint, part ofthe challenge is the timeliness of a measurement,
which is where equipment capable of making at-line
measurements really comes in to play, by helping tostreamline decision-making, and so making for a clear
return on investment.

The performance of a catalyst is dictated by morethan just what happens in the reactor initially – how
its performance changes over time is a key factor inits commercial success. Early-stage research may
not always give the answers you need, because
the performance of small quantities of well-defined
catalytic materials under ambient conditions rarelytranslates seamlessly to larger-scale conversions
under higher temperatures and pressures.
Therefore, in situ analysis of catalysts at industriallyrelevant scales over longer time-frames is a fruitfulline of enquiry for both academia and industry, andone in which Malvern Panalytical’s equipment can playa role. A further benefit of our XRF and LD systems
is that their off-line and on-line versions use thesame technology – aiding transfer of results fromearly-stage research to late-stage development.

And in addition to all this, equipment for industry needs
to be easy to use – so it’s reassuring to know that a
priority for us is ensuring that it is easy to generate sounddatasets and robust insights.
• Using raw materials responsibly and sustainably
The scarcity and price of Pt-group metals, and thedesire to source catalytic materials from sustainable,
ethical sources, is placing pressure on manufacturers
to maximize recoveries to reduce costs. Our Zetiumand Epsilon XRF instruments can assist by providing
accurate information on the abundance of highvalue elements in materials at all stages of catalyst
manufacture and recycling, helping you ensure thatyou’re making the best use of valuable materials.
• Checking that purity specifications have been met
Assessing the purity of raw materials or finishedcatalysts – or keeping an eye on composition
during manufacture – requires methods fordetermining composition that are both quick andreliable. Our Zetium and Epsilon XRF systems
provide an easy-to-learn and hassle-free wayof assessing elemental composition. Where
more detail is needed, experiments using ourEmpyrean and Aeris XRD instrument can provide
additional information on phase purity and (forexample) amorphous-to-crystalline ratios.
• Controlling particle size and shape at all stagesof manufacture
Particle size and shape distributions are fundamental
metrics of all heterogeneous catalysts, andmonitoring these is vital at all stages of manufacture,
particularly to understand the results of processing
stages such as powder mixing, nucleation,
precipitation, granulation, spray drying, calcination,
milling, extrusion or tableting. Our Mastersizer LD
system offers trouble-free monitoring of particle
size at the micro and nano- scale (and it’s alsoavailable as an on-line format, Insitec), while fornanoparticles, DLS analysis with Zetasizer is analternative option. Automated image analysis with
Morphologi (or our on-line Hydro Insight system)
additionally can spot shape anomalies that canbe a good predictor of particle flow problems.

• Predicting washcoat stability
The stability of liquid dispersion washcoats is partly
determined by the surface charge of the particles,with a high surface charge generally preventing
aggregation. The zeta potential of a surface is agood indication of surface charge, so measuring it
using our Zetasizer ELS instruments, and combining
it with knowledge of rheological properties, canbe used to optimize dispersion conditions for agiven suspension. The result? Maximum washcoatstability, and a final product with fewer defects.
• Troubleshooting during manufacture
Even the most well-controlled catalyst manufacturing
processes will occasionally run into difficulties. Whenthat happens, you need to be able to call upon arange of techniques to investigate whether there isunwanted aggregation, attrition or sedimentation, oran undesirable change in phase or surface chemistry.
Malvern Panalytical’s breadth of instrumentationcompatible with on-line or at-line analysis is your ally
when resolving a production issue. You might want
LD (Mastersizer or Insitec) to check on particle size
anomalies, XRF (Zetium, or Epsilon Xflow or Xline)
to investigate deviations in stoichiometry, image
analysis (Morphologi or Hydro Insight) to investigate
powder-flow difficulties, or XRD (Aeris) to resolve
suspected problems with structure and composition.

• Scaling-up research methods
A major challenge for catalyst researchers inacademia and industry is scaling up lab methods
to the pilot and production scales. Processes thathave worked well during the research phase may
suffer unexpected problems when scaled-up; andformulating catalysts to be mechanically stable whenpelletized is also a common challenge. Two on-line
instruments offered by Malvern Panalytical – theEpsilon (for XRF) and Insitec (for LD) – are perfectfor incorporating into scaled-up production
processes, and come complete with software
to automate measurement and analysis.
• Studying catalyst physical stability and lifetime
Under the elevated conditions of pressure ortemperature used in a reactor, the solvation
characteristics or friability of a catalyst may bequite different from that studied under less extreme
conditions during the research stage. Understanding
the mechanical stability of a catalyst is also afactor when designing the pelletization process.
The extent to which a catalyst mechanically breaks
down during use can be investigated by particle size
analysis on our Mastersizer or Insitec LD instruments,
while particle image analysis using our Morphologi
equipment can provide information on particle shape,
aiding understanding of breakdown mechanisms.

• Looking at catalysts operando
Initial research into catalyst systems often involvesa mechanistic understanding at the atomic andmolecular level. However, when applied inreal-world scenarios, the catalytic environment
may be considerably more complex. For example,
to reduce reactor downtime, a catalyst may berequired to operate under gradually changing
physical and thermal conditions. Identifying therange of acceptable reaction parameters requires
instruments that can report on key metrics insitu over time – such as our on-line Epsilon Xflow
system for elemental composition, or our on-line
Insitec LD instrument for particle size. In addition,
you can perform operando phase- or structural
analysis measurements under simulated reactor
conditions on our Empyrean XRD platform.
• Investigating recyclability
When the catalytically active metals are expensive
or in short supply, minimizing losses at every stageof the product lifecycle can have a big impact upon
profit margins. To that end, many manufacturers areinvestigating options for recycling spent catalysts,
or extracting valuable metal residues at otherstages of the production process. Understanding
the matrix in which valuable elements are present– and their levels – is a natural application ofabundance analysis using XRF, and our Zetiumand Epsilon instruments are ideal for this purpose.
The latter also has two modules (Xflow andXline) that allow on-line monitoring of elemental
composition in liquids and coatings, respectively.

8

Easy-to-perform elemental analysis
Quickly obtaining data on elemental composition
using X-ray fluorescence spectroscopy
Deviations in the chemical composition of catalysts
can have a significant impact upon final performance,
making analysis of elemental composition an
indispensable part of the manufacturing process.
X-ray fluorescence spectroscopy (XRF) is a widelyused technique for routine screening or quick analysis
of elemental composition, which does away with theinconvenience of sample digestion. It is compatible
with loose powders, pressed pellets, fused beads,
linished metals or liquids, and is also a proven method
for the mainstream assaying of precious metals.
Our XRF spectrometers, the Zetium and Epsilon ranges,
provide an easy-to-learn way to analyze elemental
composition, monitor trace elements and detect
impurities. And they’re cost-effective too, with the cost
per analysis being up to three times lower than with
ICP. Our XRF systems also excel in terms of sensitivity,with measurements of matrix element compositions andppm-level impurities being more reliable than with ICP.

9

Epsilon 4 and Epsilon 1 are compact and easy-tomaintain energy-dispersive systems that offer standalone and at-line solutions for analysis of solids andliquids. Their sensitivity can extend down to 1 ppm andbeyond, making them ideal when you need to make ameasurement during a process.
Two further Epsilon 1 instruments extend its
applicability to continuous (on-line) measurements –the Epsilon Xflow for liquids, and theEpsilon Xline for roll-to-roll coatings.
Using the Epsilon systems you'll be able to:• Measure all elements from F to Am, including alloys
and metal oxides• Obtain direct insights into production processes using
at-line elemental analysis with sample changer andautomation options• Continuously monitor deviations in stoichiometry ofslurries, as an alternative to downstream analysisof the resultant solid materials (Epsilon Xflow)• Continuously monitor reactor contents
on-line (Epsilon Xflow)• Continuously measure elemental composition duringroll-to-roll deposition processes (Epsilon Xline).

Zetium, by combining the best of wavelengthdispersive and energy-dispersive systems, offers
maximum sensitivity (down to 0.1 ppm), and issuitable for stand-alone R&D applications andprocess control across the full elemental range.

On-line XRF analysis using the Epsilon Xflow. Here, the abundance of four catalyst inhibitors in a fluid catalytic
cracking process was tracked over a period of 30 hours.

The system is stable over periods of months, meaningthat measurements don’t drift, and rendering timeconsuming re-standardizations unnecessary. Carrying out
XRF measurements is also far quicker than fire assays.

Sample preparation for XRF and ICP

Using Zetium, you’ll be able to:• Measure all elements from Be to Am,
including alloys and metal oxides• Quantify valuable elements such as Pt,
Rh and Pd in high-grade alloys• Detect low concentrations of catalyst
poisons such as Cl, S, Sn and Pb• Quickly determine metal ratios in catalytic
supports (such as Si/Al ratio in zeolites)• Carry out spot-mapping of small areas• Combine with XRD for insights into phase identity.

XRF uses fusion to create glassy sample glass discs which (unlike
analysis of powders or pressed pellets) eliminate any effects ofparticle size, mineralogy and surface roughness. Catalyst materials
are particularly amenable to fusion, and give highly reproducible
results with wavelength-dispersive XRF systems. The same sample
preparation equipment can also be used to make the peroxide or
borate solutions that are needed for ICP analysis.
Whether you’re using XRF or ICP, we can provide equipment thatwill ensure effortless sample preparation. The Claisse LeNeo is aneasy-to-use single-position instrument that is ideal for occasional or
low-throughput use. The new FORJ system, on the other hand, withcapacity for up to 12 samples, is better-suited to high-throughput
scenarios. It’s also the world’s fastest, safest and most accurate fusion
instrument for sample preparation, designed for minimal maintenanceand repeatability of results.
Did you know? We also provide certified reference materials (CRMs),
together with the expertise you need to set up bespoke calibrations
and standard operating procedures.

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11

High-resolution particle size distributions
Obtain new insights with precision analytical instrumentation

The Insitec system is tailored to on-line monitoring,
providing real-time analysis every few seconds
for powders, emulsions, sprays and slurries over a
specified size range (lenses are available for bands
covering the size range 0.1–2500 µm). This makes
it ideal for fast-moving production environments,
facilitating quick remedial action, and so helping to
reduce waste and make workflows more efficient.

Using Insitec, you’ll be able to do many of themeasurements you can do on the Mastersizer, plus:• Obtain direct insights into production processes
using on-line size analysis (and you can use
Insitec alongside Epsilon Xflow or Epsilon Xline
for on-line elemental abundance information)• Troubleshoot suspected particle
size issues during milling• Check particle size evolution overtime during sedimentation.

Optimizing the particle size distribution is central to several stagesof catalyst production, from the preparation of precipitates, powders
and washcoats to the molding of the final catalyst block.
To meet this diversity of needs, two easy-to-use instruments
are offered by Malvern Panalytical for measuring particle
size – the Mastersizer 3000 and the on-line Insitec system.
Both employ the technique of laser diffraction, which unlike
grindometers provides information on the overall size distributionof catalyst particles, not just the largest particles present.
In addition, because the data represents the properties of thewhole material, the results are statistically superior to microscopy(which depends upon selecting a representative sample). Laser
diffraction is also high-resolution, easy to perform and operatorindependent, making it useful to replace or complement othermethods (for example, those used for benchmarking or calibration).

As the process requirements are changed and the
manufacturing feed lines are adjusted, successive
measurements in a 1 hour period track the change
from coarse (red) to fine (black) precipitated calcium
carbonate powder.

Understanding nanoparticle distributions using
dynamic light scattering

The Mastersizer 3000 delivers rapid, accurate
particle size distributions for powders, suspensions
and emulsions over the size range of 0.01–3500 µm– making it a dependable and versatile instrument
for the majority of particle sizing applications.

Laser diffraction is ideal for the vast majority of catalyst
applications, but when the particles being researched
are below 600–800 nm (as, for example, in some highlydispersed colloids), dynamic light scattering (DLS) offers
greater sensitivity, and below 200–300 nm becomes therecommended option.

And with a small footprint, plus effective sample
preparation capabilities, flexible reporting, andoptions for process automation, Mastersizer
3000 is guaranteed to be a success in the
research lab and on the production line.

Moreover, because DLS systems are far less expensive
and more user-friendly than transmission electron
microscopy, they are ideal for researchers needing
to routinely and quickly measure size distributions inthis range.

Using Mastersizer 3000, you’ll be able to:• Quickly and easily obtain high-quality,
reliable data about particle size

Using Zetasizer Advance systems, you’ll be able to:• Quickly and easily obtain high-quality,
reliable data about nanoparticle size
• Control nanoparticle precipitation – for example,of precious metal nanoparticles in a washcoat• Maximize the shelf-life and efficacy of washcoats
for nanoparticle absorption onto substrates• Predict issues with particle agglomerationor settling before they happen.

The Zetasizer Advance range are the most widely used
instruments for measuring both particle size and zetapotential. Ask about our MADLS® technology and how it
uses advanced algorithms to combine multi-angle datafor greater sensitivity and precision!

• Check the size of precipitates and post-milled
powders, particularly to avoid over-milling• Estimate the specific surface area (SSA) of catalyst
supports (note that values tend to be smaller
than obtained with BET measurements, which
are sensitive to the internal pore structure)• Control particle size in washcoats (whatever thesolvent system), and so optimize their impregnation
into (or adhesion onto) catalyst supports• Optimize the rheology and compressibility of thecatalytic powder at the final shaping stage• Use pressure titrations to understand the riskof catalyst attrition in fluidized-bed reactors.

Using Mastersizer 3000, size distributions for three
Pt loading levels on Vulcan XC-72 carbon black were
accurately generated, showing a bimodal distribution
for the lowest loading.
Intensity size distribution as measured by MADLS®
of gold nanoparticles. Further measurement using
polarized light revealed that the smaller peak arosefrom rotation of some elongated particles.

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Statistically-sound particle
shape analysis

Reliable zeta potential measurements

Acquiring detailed particle morphology
data using image analysis

Unpacking the role of surface charge using
electrophoretic light scattering

Particle shape is a complex topic in catalyst
manufacture, but one that is important tounderstand because of its numerous effects onprocessing and (ultimately) catalytic activity.

In catalyst manufacture, the charge on particles
has an important role to play in adhesion andaggregation processes, and this propensity to develop
a charge can be quantified by the zeta potential
using electrophoretic light scattering (ELS).

The manual microscopy methods historically used
to analyze shape were highly time-consuming, andhave now been superseded by automated image
analysis, for example using our Morphologi 4 andHydro Insight instruments. This automation alsomeans that analysis can be performed on large
sample sets – typically 10,000 to 500,000 particles.

Morphologi 4 uses automated static image analysis
to provide data on over 20 morphological particle
parameters, for dry powders, wet suspensions andparticulates collected on filters, in the range 0.5 to>1300 µm. Moreover, SOP control and software filters
ensure robust, repeatable measurements, even for
low-contrast particles, or where small fragments,
image anomalies or touching particles are present.
Using Morphologi 4, you’ll be able to:• Obtain highly detailed, statistically robust
particle shape and size distributions• Obtain information sphericity/irregularity or
the presence of anomalous particles• Study the microstructural propertiesof carbon materials (which are often
used as metal-free supports).

To enable catalyst manufacturers to accurately
measure zeta potential, we offer the Zetasizer Advance
range of instruments – the successor to the highly
successful and market-leading Zetasizer Nano.

Partial catalog of a 40% Pt/C catalyst powder used in a catalytic
ink imaged by Morphologi 4. Although the agglomerates areroughly spherical, their roughness could affect the ease ofdispersion in the ink and the formation of porosity during
deposition and drying.

Hydro Insight is a dynamic imaging accessory
for wet dispersions that sits alongside theMastersizer 3000 (see page 10), and which can
image suspended particles at up to 127
frames per second, and so provide realtime information on particle shape.

The Zetasizer Advance range of instruments is ideal
for measuring zeta potential with excellent accuracy,
repeatability and consistency in process or laboratoryenvironments.

Zetasizer's multipurpose titrator MPT-3 allows you to set
up titrations in different ways to suit your sample and findthe optimum pH for stability.

When highly conducting samples are being studied,Zetasizer has you covered, with ‘constant-current zeta’technology keeping the current unchanged even whenions build up on the electrodes, and the mixed-mode‘M3-PALS’ method avoiding distorted results caused byelectro-osmosis.

• Find out everything you need to know about
zeta potential of your particle dispersion

Because all colloidal samples are different, theUsing Zetasizer Advance, you’ll be able to:• Understand the root causes of unstable particle
dispersions or poor particle adhesion• Optimize aggregation of catalytic powders, toaid compressibility for tableting/extrusion• Optimize formulation stability by titration against
pH or concentration of steric dispersant• Ensure optimized distribution of active sites
following active-material impregnation.

Using Hydro Insight, you’ll be able to:• Acquire on-the-spot information on
particle shape in wet dispersions• Respond rapidly to an imperfect batch• Troubleshoot issues arising duringmethod development.

With Hydro insight, powerfulimage processing software
analyses successive highresolution frames, presenting
histograms of parameters, suchas the size class histogram
shown here.

The formation of large particles due to aggregation andflocculation is enhanced when the net charge of theparticles is close to zero. The pH of a dispersion can bechanged to prevent floculation and achieve stability.

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15

Powerful phase analysis
Investigating catalyst phases in unmatcheddetail using X-ray diffraction

The Empyrean range of instruments areversatile, sophisticated platforms that offer
the widest possible choice of measurements,
meaning you’re literally ready for anything.
Ideally suited to R&D laboratories, Empyrean is the
only XRD system with the ability to measure all sample
types on a single instrument. And with automatedMultiCore optics, switching between measurement
or sample types is easier than ever before.
Using Empyrean, you’ll be able to do
everything you can with Aeris, plus:• Have access to the widest possible range of
XRD experiments, for unparalleled flexibility• Carry out extensive operando or in-situ
measurements on catalytic materials,
for real-world insights• Determine the larger dimensions (andpore sizes) of catalyst scaffolds using
small-angle X-ray scattering (SAXS)Understanding the atomic structure of crystalline
phases is an essential part of determining the structure–
performance relationships and reaction mechanisms ofheterogeneous catalysts, and X-ray diffraction (XRD) has
long been valued by materials scientists for this purpose.

2500

Using Aeris doesn’t require expertise in XRD. And withthe option of belt automation, sample processing iseasily scaled up, with a typical sample taking justa few minutes – helping you improve production
efficiency, reduce costs and control the quality of
the finished product. In addition, expertise packages
can be employed to set up fully automated phasecomposition results for your routine samples, so thatyou can streamline your QC and trend analysis.

2000

Using Aeris, you’ll be able to:

Two XRD instruments from Malvern Panalytical arevalued by those in the catalyst industry for the
analysis of catalyst materials: Aeris and Empyrean.
5 Minute scans
MOF CAU-10H synthesis 1

Intensity (counts)

Aeris is a compact diffractometer offering industryready measurement and data analysis on avariety of powder diffraction configurations.

MOF CAU-10H synthesis 2

SAXS measurements of pure Fe2O3 and PdO/Fe2O3
nanoparticles, carried out on Empyrean, showing an
R50 value of about 20 nm in both cases, but with abroad size distribution. The derived specific surface
area for PdO/Fe2O3 is slightly larger than the(BET-validated) value for Fe2O3, as would be
expected from the presence of active surface sites.
Sample courtesy of TU Vienna, Austria.

• Automate the routine quantification ofphases (e.g. γ-alumina, zeolites)

1500

1000

• Measure the degree of crystallinity of active phases

5000• Understand the local structure of amorphousmaterials using X-ray total scattering andpair distribution function (PDF) analysis.

7

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9

10

11

12

13

14

15

16

17

18
2Theta (°)

To refine your processing parameters, you need toanalyze them quickly. With Aeris, even five-minute scans
can immediately show whether a processing parameter
is affecting crystalline phase purity. This figure shows
two five-minute measurements of two metal-organic
framework (MOF) samples in reflection mode, eachprocessed under different conditions. Using Aeris, you
can rapidly optimize these processing parameters for thebest quality material – every time.

Ask us about the new in-situ
catalyst cells!

• Determine the point of termination of thecrystallization step during manufacture• Combine phase information with XRF datafor insights into element distribution• Carry out grazing-incidence measurements toimprove data quality for surface layers and coatings• Carry out transmission XRD measurements at
low angles, to study microporous materials.

In-situ monitoring of the thermal response of catalystmaterial Fe2O3 and PdO/Fe2O3 between 250°C and
800°C using an Anton Paar HTK 1200N stage on
the Empyrean platform. (a) A stack plot of XRD data
files shows a phase transition from maghemite tohematite. (b) An isolines plot for the two Fe2O3 phases
indicates this phase transition takes place at around
450°C. (c) An isolines plot for PdO/Fe2O3 shows asharpening of the primary peak corresponding to PdO
at approximately 550°C, indicating an increase in the
average crystallite size of PdO and loss of the small
surface domains on the support material.

The X-ray diffraction peaks of nanoparticles can bevery broad, preventing the accurate determination oflattice parameters, but models based on pair distributionfunction (PDF) data, acquired on Empyrean, can beused to derive useful information. (a) PDF for CeO2
nanoparticles; (b) the PDF-derived plot of the cubic CeO2
lattice parameter, shown as a function of synthesis time.
The value increased for the first 15 hours, indicating that
active particle growth is taking place.

We draw on the power of our analytical instruments
and services to make the invisible visible and theimpossible possible.
Through the chemical, physical and structural analysis
of materials, our high precision analytical systems andtop-notch services support our customers in creating abetter world. We help them improve everything from theenergies that power us and the materials we build with,to the medicines that cure us and the foods we enjoy.
We partner with many of the world’s biggest companies,
universities and research organizations. They value us
not only for the power of our solutions, but also for thedepth of our expertise, collaboration and integrity.
We are committed to Net Zero in our own operations
by 2030 and in our total value chain by 2040. This is
woven into the fabric of our business, and we help our
employees and customers think about their part increating a healthier, cleaner, and more productive world.

Service & Support
Malvern Panalytical provides the global training, service
and support you need to continuously drive youranalytical processes at the highest level. We help you
increase the return on your investment with us, andensure that as your laboratory and analytical needs
grow, we are there to support you.
Our worldwide team of specialists adds value to yourbusiness processes by ensuring applications expertise,
rapid response and maximum instrument uptime.
• Local and remote support• Full and flexible range of support agreements• Compliance and validation support• Onsite or classroom-based training courses• e-Learning training courses and web seminars• Sample and application consultancy

With over 2300 employees, we serve the world, and weare part of Spectris plc, the world-leading precision
measurement group.

Malvern Panalytical. We’re BIG on small™

Malvern Panalyticalwww.malvernpanalytical.com

Grovewood Road, Malvern,
Worcestershire, WR14 1XZ,
United Kingdom

Lelyweg 1,7602 EA Almelo,
The Netherlands

Tel. +44 1684 892456
Fax. +44 1684 892789

Tel. +31 546 534 444
Fax. +31 546 534 598

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Copyright: © 2023 Malvern Panalytical. This publication or any portion thereof may not be copied or transmitted without our express written permission. PN13757

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