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DISCOVERY HYBRID RHEOMETER

Discover the
rheometer
with the
Sensitivity
Ease-of-use
Versatility

to address the most


demanding applications
HR 30/20/10 DISCOVERY HYBRID RHEOMETER The DISCOVERY HYBRID RHEOMETER
The MOST POWERFUL and VERSATILE RHEOMETER
for your laboratory
TA Instruments invites you to experience the latest innovations in rotational shear rheometers, the Discovery
Hybrid Rheometer HR 10, HR 20, and HR 30. The Discovery Hybrid Rheometers are designed for scientists who
need to obtain better rheological data, under the widest range of measurement conditions, collected by more
users, with less training.

Advances in core measurement technology enable more sensitive measurements with superior
precision. This empowers you to measure lower viscosities and weaker liquid and soft-solid structure,
while consuming less material. Superior dynamic performance gives a higher level of accuracy in
measurements of G’ and G” so you can make decisions quickly, with confidence.

Thoughtful hardware and software design results in a complete system that simplifies every user
interaction. Routine functions are faster and more intuitive, so you can accomplish more with less
training.

The performance of the Discovery Hybrid Rheometer is supported by the widest range of powerful,
easy-to-use environmental systems and accessories that allow you to replicate demanding
environmental conditions, incorporate complementary simultaneous measurements, or extend your
rheometer beyond conventional shear rheology.

Discover the advanced engineering and attention to detail that provides enhancements in every aspect of
rheometer technology and user experience. From the most cost-effective rheometer with industry-leading
performance to the most advanced rheometer available, there is a Discovery Hybrid Rheometer to meet your
needs and exceed your expectations.

2 The Discovery Hybrid Rheometer 3


Optic
al E
nc
od
aring er
u s t Be
Thr

Du
tic
DISCOVER ne

al
ag

Re
ad
M
UNPARALLELED MEASUREMENT

er
SENSITIVITY and ACCURACY
Measure the lowest stresses and smallest sample volumes with
revolutionary torque sensitivity
Unrivaled low torque sensitivity empowers you to measure lower viscosities and weaker intermolecular structures
while using lower sample volumes.

All Discovery Hybrid Rheometers feature TA’s patented Magnetic Thrust Bearing, which reduces basic system
Report G’ and G” with confidence
friction by 70% compared to traditional designs. By eliminating the contributions of high-pressure turbulent air
flow from the measurement system, lower torques can be measured reliably and accurately. The storage and loss modulus, G’ and G”, are two of the most insightful
up
gC
measurements provided by any rheometer.
a
The unparalleled sensitivity of the magnetic thrust bearing is coupled with the NEW improved Advanced Drag Dr
d The Discovery Hybrid Rheometer’s exclusive Optical Encoder Dual Reader
Cup Motor. Enhanced torque precision increases the accuracy of every measurement, especially at low torques.

e
nc
improves phase angle precision by 70% compared to conventional single-

va
reader designs. This leads directly to a more accurate measurement of

Ad
The measurement you want: Advanced Strain and Stress Control G’, G”, and tan δ. This advantage becomes most evident under challenging
experimental conditions such as low stresses, small strains, or difficult samples
The Discovery Hybrid Rheometer performs the experiment you want, whether stress-controlled, strain-controlled,
that exhibit only trace amounts of damping or elasticity. The Optical Encoder
or both. State-of-the-art high-speed electronics and the responsive Advanced Drag Cup Motor provide the
Dual Reader also provides a 5× improvement in displacement resolution,
fastest transient responses and accurate control in any type of deformation. Direct Strain oscillation provides
permitting more accurate measurements at lower strains.
real-time strain control at every point of the oscillatory measurement.

Responsive strain control ensures rapid data collection so you can characterize materials that are undergoing The Advanced Drag Cup Motor is optimized for accuracy in dynamic
thermal, chemical, or structural transitions. Highly accurate deformation control (stress or strain) also ensures measurements. The low-mass and -radius design reduces system inertia by
the highest data quality, particularly when evaluating materials that show a non-linear response at very large up to 80% compared to DC motors, minimizing corrections to oscillation data,
amplitudes. especially at higher measurement frequencies. The result is a wider range
of accurate measurement frequencies, material types, and experimental
(US Pat. 7,137,290; 7,017,393; 6,798,099)
designs.

4 5
ce Rebalance
a l For Tra
N orm ns
d uc

MEASURE the STIFFEST MATERIALS


e

r(
FR
) T
with CONFIDENCE and ACCURACY Rigid Cast Aluminum Frame

The Discovery Hybrid Rheometers are designed with Advancing Every Aspect of the
sensitivity to measure the softest materials, and are Rheological Measurement
constructed to be rugged enough to handle the
True Position Sensor
stiffest materials and toughest users.
arings
The DHR includes the patented True Position Sensor (TPS) for true gap
ia l Be
accuracy. The TPS is a high-resolution linear position sensor that measures d
A rigid cast aluminum frame and rugged linear ball slide provide more Ra
than 60% greater axial and torsional stiffness than other designs and and compensates for the effects of thermal expansion in real time.
permit gap position resolution of 0.02 µm. Unlike competitive devices, the TPS eliminates errors associated with
thermal expansion without the need for special high inertia iron core
ion Sensor (TPS)
Two high-stiffness radial bearings stabilize the system from side loads geometries and environmental systems. o s it
ueP
exerted by samples or operators while the Optical Encoder Dual Reader Tr
further cancels displacement measurement drift associated with testing The TPS works with all Smart Swap™ geometries and Smart Swap™
very stiff samples over long times. environmental systems.
(US Pat #10,161,843)

The Advanced Drag Cup Motor provides stable control and measurement
even when operating under extreme conditions. Active and passive Normal Force Rebalance Transducer (FRT)
thermal systems manage heat and account for system temperature,
The Force Rebalance Transducer is the premier technology for normal force
guaranteeing measurement accuracy under all test conditions.
measurements. This active, non-compliant device accurately measures
normal and axial forces without deflection. Competitive capacitive or
These innovations provide the most accurate and sensitive measurement,
strain gauge sensors rely on physical movement of the device to sense a
under even the most extreme experimental conditions.
force, resulting in measurement error. The FRT provides the most accurate
normal force measurement by driving the linear motor to maintain zero
deflection at all times and conditions. The FRT also works in conjunction
with the magnetic thrust bearing to enable axial DMA capability.

(US Pat #6,798,099)

6 7
DISCOVER the RHEOMETER 0 ° Sa
mple Stage L
igh Smart Sw
36 tin

that WORKS WITH YOU


g ap
ed ™
at G
e

r
eg

om
Int

et
rie
s
The NEW Discovery Hybrid Rheometer is your Versatility is being ready to face whatever the day brings. Whatever
that may be, the NEW Discovery Hybrid Rheometer will be ready. The
invisible partner in the lab, reducing the time from
Discovery Hybrid Rheometer features the widest range of powerful,
question to insight. easy-to-use environmental systems and accessories that allow
you to replicate demanding environmental conditions, incorporate
complementary simultaneous measurements, or extend your rheometer
Load samples with confidence and ease beyond conventional shear rheology.
The Discovery Hybrid Rheometer is designed by rheometer users
to make sample loading faster, easier, and improve measurement Smart Swap™ Geometries
precision for every operator.
The NEW Smart Swap 2™ geometry system features an all new system Smart Sw
for optical information storage and transfer. This system provides greater ap
Expedite routine interactions with a gap positioning system that is Te
storage and durability than chip-based systems. When attached,
m
3× faster than other rheometers while maintaining a 0.02 µm gap p
the complete geometry information, including unique dimensions is

er
resolution. A convenient tactile keypad places the most common

at
automatically detected and the software is appropriately configured.

ure
actions where you need them most, including thoughtful features like
automated trim gap, measurement position, and bearing lock. Convenient Tactlie

Sys
Smart Swap Temperature Systems Keypad

tems & Accesso


Even more power is offered by the new One-Touch-Away™ app-style and Accessories
touchscreen that greatly enhances usability by placing key instrument
Only TA Instruments offers the convenience and versatility
features at your fingertips.
of Smart Swap temperature control options and accessories.
Smart Swap options are attached to the instrument on its unique
Every user will appreciate the brand new integrated 360° sample stage
magnetic base, providing faster, easier installation than mechanical
lighting that enhances visibility in any lab environment. The result is

ri e
systems. Once attached, the instrument automatically detects and

s
easier, more repeatable sample loading and trimming, leading to
configures the system for operation.
improved data accuracy and precision.

8 The Discovery Hybrid Rheometer 9


DHR DYNAMIC MECHANICAL ANALYSIS (DMA) 3-Po
int Bending d (C
antilever)
Be
Tension Compression
pe n di
m
la n
C

g
Backed by over four decades of TA Instruments’ expertise
in rotational rheology and linear DMA measurements,
the Discovery Hybrid Rheometer’s DMA Mode adds a
new dimension for testing solid and soft-solid materials.
Now in addition to the most sensitive and accurate
rotational shear measurements, the DHR can deliver
accurate linear Dynamic Mechanical Analysis (DMA)
ABS bar - Cantilever 3 mm x 12.75 mm x 25 mm PET Film - Tension 50 µm thick
data. Controlled axial oscillations permit the direct
measurement of E’, E”, and tan δ in tension, bending and 1010 102 1010 103
compression, a perfect addition to shear measurements,
including solids in torsion. The new DMA mode is ideal
109 101 109
for identifying a material’s transition temperatures and
102
provides reliable measurements over the instrument’s full

E”(Pa)

E”(Pa)
range of temperatures.

tan(δ)
108 100 108

tan(δ)
101
The axial DMA capability is enabled by the DHR’s
107 10-1 107

E’(Pa)
active Force Rebalance Transducer (FRT) and patented

E’(Pa)
magnetic bearing technologies that permit amplitude-
100
controlled oscillatory deformation in the axial direction. 106 10-2 106
Installation of external components is never required, so it
is always quick and easy to get great data! Competitive
105 10-3 105 10-1
instruments that employ air bearings and passive normal -100 -50 0 50 100 -100 -50 0 50 100 150 200 250
force measurements are inherently incapable of such Temperature (˚C) Temperature (˚C)
measurements without costly modifications.

The figure above demonstrates the performance of the DMA mode during a temperature Axial DMA tests on thin films require maintaining the axial force above the oscillation
Every Discovery Series HR 30 rheometer ramp of an acrylonitrile butadiene styrene (ABS) sample in single cantilever from force to hold the sample in tension throughout the test. This capability is highlighted in
includes this DMA capability and -100 °C to 140 °C. Two major transitions corresponding to the individual glass transitions the plot above, showing the results of a temperature ramp on a 50 μm thick PET film tested
it may be added to any HR 20. of the styrene (-82 °C) and butadiene (115 °C) components are evident, indicating the using the tension geometry over a temperature range of -100 °C to 250 °C. Three major
incompatibility of the two monomers. transitions are observed: a beta glass transition at -80 °C, an alpha glass transition at
about 111 °C, and a melt at 236 °C. The data reveal a semi-crystalline structure with two
amorphous relaxations and the DHR’s force-tracking capabilities at work.

10 The Discovery Hybrid Rheometer 11


TECHNOLOGY “APP” STYLE TOUCHSCREEN

Revolutionary rheometer performance at your The app-style touchscreen includes:


fingertips • Start/stop experiments
The new Discovery Hybrid Rheometer boasts a brand-new One-Touch-Away™ • Set temperature
app-style touchscreen that greatly enhances usability by placing key instrument • Set gap
features at your fingertips. • Controlled rotation for sample loading
• Procedure and sample details
• Ergonomic design for easy viewing and operation • Real-time signals
• Packed with functionality to simplify operation and enhance user experience • Test and instrument status at a glance
• User prompts

The app-style touchscreen, powerful new TRIOS software, and quick robust
calibration routines work seamlessly to dramatically improve laboratory
workflows and productivity.

12 The Discovery Hybrid Rheometer 13


TECHNOLOGY TRIOS SOFTWARE
The Most VERSATILE CONTROL
TA Instruments’ state-of-the-art software package uses cutting-edge technology for instrument
control, data collection, and data analysis for thermal analysis and rheology. The intuitive user
and ANALYSIS SOFTWARE!
interface allows you to simply and effectively program experiments, and move easily between
processing experiments and viewing and analyzing data. Complete Data Analysis Capabilities
A comprehensive set of relevant tools are available for real-time data analysis, even during
experiments. Gain actionable insights into your material behavior through a powerful and versatile

TRIOS Features: Complete Data Record set of features seamlessly integrated into TRIOS.

• Control multiple instruments with a single PC and software package The advanced data collection system automatically saves all relevant signals, active
All Standard Analyses
calibrations, and system settings. Waveforms for each data point may be displayed as
• Overlay and compare results across techniques including DSC, TGA, DMA, SDT, • Onset and endset analysis
Lissajous plots and provide a visual representation of the stress-strain relationship. This
TMA and rheometers
comprehensive set of information is invaluable for method development, procedure • Signal maximum and minimum
• Unlimited licenses and free lifetime software upgrades deployment, and data validation. • Signal change
• One-click repeated analysis for increased productivity • Modulus crossover
• Automated custom report generation including: experimental details, • Curve values at specific X or Y points
data plots and tables, analysis results • 1st and 2nd derivatives
• Area under the curve
• Convenient data export to plain-text, CSV, XML, Excel®, Word®, PowerPoint®,
and image formats • Peak height
• Peak integration and running integral
• Optional TRIOS Guardian with electronic signatures for audit trail and data
integrity including U.S. FDA 21 CFR 11 compliance
• Mathematical fitting: straight line, polynomial, or exponential
• Statistical functions

Advanced Analysis Capabilities


TRIOS Software provides the right experience
for every user • More than 10 flow models including automatic model selection based on
best fit to experimental data
• Viscoelastic transformations to interconvert between oscillation, stress
relaxation, stress growth, creep, relaxation spectra, retardation spectra, and
TRIOS for the Discovery Hybrid Rheometer features two powerful user interfaces memory functions.
• Time-Temperature Superposition (TTS) analysis with automatic curve shifting
that present users with what they need to collect the data they want. and Mastercurve generation • Advanced custom analysis with user-defined variables and models
• Activation Energy calculation • Cox-Merz: η*(ω)→ η( )
TRIOS Express helps users to design the most common measurements quickly
• WLF coefficient calculation • Fluid Inertia Correction
and easily. Simple forms and sensible defaults streamline the process of
• Convert between temperature ramps and frequency sweeps • Rabinowicz Correction
experiment design and execution.
• Cole-Cole, Van Gurp-Palmen, and Lissajous plots • Direct Creep – Oscillation conversion
TRIOS Unlimited gives you complete control. A robust set of detailed experimental • Built-in models for: discrete and continuous relaxation or retardation spectra, • Discrete Fourier Transformation (DFT)
controls and data collection options ensures that you will be able to design the Oldroyd and Spriggs models
• Window Correlation
experiment you envision and collect the data you need. • Creep ringing analysis by Kelvin, Maxwell, or Jeffreys models

14 The Discovery Hybrid Rheometer 15


TECHNOLOGY AUTOPILOT SOFTWARE Guided Operation
AutoPilot allows for guided operation of the Discovery Hybrid Rheometer. Utilize available audio and video
playback capability and interactive prompts to instruct users on proper operational techniques.

Experience a new paradigm in software functionality and unleash the full potential of your • Simple message boxes provide basic text feedback
Discovery Hybrid Rheometer with AutoPilot, a premium feature that enables complete automation • Prompt operators for experiment parameters
of powerful TRIOS software. AutoPilot allows users to quickly and easily create automated routines; • Play videos to show proper sample loading, trimming, and cleaning technique
from test methods to data analysis and report generation. These routines empower laboratories • Play sounds to provide audible indicators during script execution

to streamline and standardize operations and decision-making across local or global laboratory • Timers provide visual indication of time remaining in current step

enterprises. From quality control to research and development, laboratory environments of all
types will benefit from increased productivity, improved data precision, and reduced training time. Unlimited Power
AutoPilot provides the ability to automate all the powerful TRIOS functions like data analysis and report
generation, plus instrument actions like calibrations and temperature and gap commands. With more than 100
Simplified Interface programmable operations, users can:
AutoPilot includes a customizable TRIOS ribbon and One-Touch, a simplified single-click PC user interface. Save time by centrally locating
• Monitor live signal values to detect loading errors or dynamically change test parameters
standard operating procedures (SOPs) in the configurable One-Touch layout. Quickly execute common tasks using custom TRIOS ribbon
buttons. With a single click, operators will be able to reliably and repeatably execute complex procedures. • Load existing data sets for processing and trend analysis

• Create overlays, generate reports, and populate control charts


• One-Touch interface provides easy organization and execution of scripts
• Automate decision-making on processed data
• Increase efficiency and productivity using custom ribbon buttons to repeat routine tasks

• Personalized button settings provide easy recognition of script functionality


Intuitive Programming
AutoPilot scripts are built using Blockly, a visual programming interface developed by Google. The drag and drop
constructs enable effortless script creation. Perform complex tasks out of the box using the included example
scripts or create your own using Quick Steps and Express Scripts preconfigured routines that enable the rapid
development of intricate procedures.

• Color-coded, puzzle-piece programming

• Requires little or no training

• Progressively grow your capabilities using the included examples and built-in Quick Steps and Express Scripts
LIMS/NOTEBOOK
LIMS Compatibility
AutoPilot provides a seamless mechanism for integration into any LIMS system. Programmatically export raw data
.txt
for incorporation by any third-party. Out-of-the-box supported formats include .txt, .xml, and .xls.
.xml
.xls

16 The Discovery Hybrid Rheometer 17


DHR TEMPERATURE SYSTEMS
The World’s most Versatile platform
All DHR temperature systems and accessories are designed with superior performance and ease-of-use in mind. Only
TA Instruments’ DHR offers the convenience and versatility of Smart Swap™ geometries, temperature systems, and accessories. for Rheological Measurements
Smart Swap technology provides fast and easy interchange of accessories with automatic detection and configuration
of the rheometer for operation.

Electrically Heated Concentric Electrically Heated Plates, EHP Dual Stage Peltier Plate Upper Heated Plate, UHP
Peltier Plate Peltier Concentric Cylinder Cylinder Provides active heating and cooling of cone and The Dual Stage Peltier Plate is another first from the The UHP is a temperature option designed for use with

Our best-selling temperature control system The DHR patented Peltier Concentric Cylinder The new Electrically Heated Concentric Cylinder parallel plate geometries to a maximum temperature of innovator of Peltier Plate technology. The unique design Peltier plates to help ­minimize vertical temperature

is the Peltier Plate. It can handle the widest combines the convenience of Smart Swap and Peltier (EHC) system extends the temperature of concentric 400 °C. Optional Gas Cooling Accessory extends uses a stacked Peltier element approach. The benefit gradients. The UHP is compatible with all Peltier plate

range of material applications with standard, heating technology with a wide variety of cup and cylinder measurements to 300 °C. Efficient electrical the temperature to -70 °C. The EHP is ideal for high- is unprecedented low temperature performance models and provides both upper plate temperature

stepped, and disposable models. Temperature rotor geometries. Concentric cylinder geometries heaters and optimized heat transfer ensure the most throughput polymer sample testing. With patented providing a continuous temperature range of control and purge gas environment. The UHP has

range is -40 °C to 200 °C with controllable heating rates are commonly used for testing low viscosity fluids, accurate and uniform temperature control. The EHC is Active Temperature Control, (ATC),­­­it is the only EHP -45 °C to 200 °C with water circulating at a single a maximum temperature of 150 °C and the lower

of up to 20 °C/min. Peltier Plate accessories include dispersions or any liquids that are pourable into a cup. compatible with a wide variety of concentric cylinder system capable of direct temperature control of the heat sink temperature. The Dual Stage Peltier is the temperature can be extended using liquid or gas

evaporation blocking, thermal covers, purge covers, Convenient Peltier technology provides stable and accessories, including the popular Pressure Cell. upper and lower plates. Standard and disposable perfect choice for applications requiring sub-ambient cooling options. The UHP is the only non-contact

and immersion capability. It is the highest performing, responsive temperature control from -20 °C to 150 °C. systems are available for polymer melt and temperature control. temperature system to feature patented Active

most versatile, and best accessorized Peltier Plate (Patent # 6,­­­­588,254) thermosetting materials. A camera viewing option is Temperature Control for direct measurement and

temperature system on the market. available. control of the upper plate temperature.

18 The Discovery Hybrid Rheometer 19


DHR ACCESSORIES

Environmental Test Chamber (ETC) Air Chiller Systems (ACS-2 and ACS-3) Relative Humidity Accessory
The ETC is a high temperature Smart Swap TM
oven that uses controlled convection/ The new Air Chiller Systems are unique gas flow cooling systems The DHR-RH Accessory is a new environmental system that
radiant heating. Temperature range is -160 °C to 600 °C with heating rates up to 60 °C/ that enable temperature control of the Environmental Test Chamber enables accurate control of sample temperature and relative
min, providing fast response and temperature stability. The ETC is a very popular option for without the use of liquid nitrogen. Equipped with multi-stage humidity. The accessory employs a custom-designed humidity
polymer applications and can be used with parallel plate, cone and plate, disposable plate, cascading compressors, the ACS-2 and ACS-3 permit operation of and temperature chamber that is optimized for rheological
rectangular torsion, and axial DMA clamps for solids. Image capture and camera viewing the ETC at temperatures as low as -50 °C and -85 °C, respectively. measurements and provides stable, reliable control of temperature
is optionally available over the entire temperature range. Utilizing compressed air, the Air Chiller Systems can help eliminate and humidity over a wide range of operating conditions.
or reduce liquid nitrogen usage from any laboratory and offer an A wide variety of test geometries are available, including
incredible return on investment. geometries specially designed to study true humidity-dependent
rheology.

20 The Discovery Hybrid Rheometer 21


DHR ACCESSORIES

Advanced Peltier Plate


The Advanced Peltier Plate combines ultimate flexibility
with exceptional temperature performance in a single
Peltier Plate temperature system designed to cover
the widest range of applications. The unique Quick
Change Plate system provides the ability to easily attach
lower plates of different materials and surface finishes,
disposable plates for testing curing materials, and an
Immersion Cup for characterizing materials in a fluid
environment.
­Solvent Trap/Evaporation
Blocking System Insulating Thermal Covers Purge Gas Cover
Solvent Trap cover and Solvent Trap geometries together Thermal Insulation Covers are constructed of an anodized The Purge Gas Cover is a hard-anodized aluminum two-
create a thermally stable vapor barrier, virtually eliminating aluminum core surrounded by an insulating exterior. The piece split cover with 4 mm diameter compression fittings.
any solvent loss during rheological experiments and aluminum core conducts heat to the upper geometry, This cover can be used to purge the sample area with
improving temperature uniformity. ­ providing uniform temperature throughout the sample. dry nitrogen gas to prevent condensation below room
Insulated Solvent Traps offer the added benefit of temperature, or purge with humidified gas to prevent
preventing evaporation. sample drying.

22 The Discovery Hybrid Rheometer 23


DHR ACCESSORIES

Optics Plate Modular Microscope ­Small Angle Light


Accessory (OPA) Accessory (MMA) Scattering (SALS) Rheo-Raman Accessory
The OPA is an open optical system The MMA enables complete flow The SALS option provides simultaneous The new Rheo-Raman Accessory allows
that permits basic visualization of visualization with simultaneous rheological and structural information for simultaneous collection of Raman
sample structure during rheological rheological measurements. A high- such as par ticle size, shape, spectroscopy data during rheology
experiments, revealing important insights resolution camera collects images at up orientation, and spatial distribution. experiments. Raman spectroscopy
Interfacial Rheology: Double Wall Ring and Double Wall Du Noüy Ring Interfacial Exchange Cell
about material behavior under flow. An to 90 fps coupled with industry-standard The accessory features patented is a technique that provides critical Patented technologies allow the characterization of interfacial rheology using specialized geometries to measure The new Interfacial Exchange Cell expands
open platform with a borosilicate glass microscope objectives that provide Peltier Plate temperature control, information about molecular structure the viscosity and viscoelastic properties at two-dimensional liquid-air and liquid-liquid interfaces. The well-defined TA Instruments’ patented offerings for interfacial
plate provides a transparent optical magnification up to 100×. Illumination scattering angle (θ) range of and bonding and can elucidate flows and negligible subphase contributions in the Double Wall Ring (DWR) and Double Wall du Noüy Ring (DDR) rheology by providing the ability to directly
path through which the sample can from a blue-light LED can be combined 6° to 26.8°, scattering vector range (q) intermolecular interactions of pure make these tools the preferred choice for sensitive measurements of interfacial rheology. In TA Instruments interfacial manipulate the composition of the lower liquid layer
be viewed directly. This enhances the with a cross-polarizer or dichroic splitter of 1.38 μm to 6.11 μm . Length scale
-1 -1
components and mixtures. The Rheo- rheology systems, the sample is contained in a Delrin trough with measuring geometries made of Platinum-
®
(subphase) during rheological measurements. This
understanding of a range of materials, for selective illumination or fluorescence range is 1.0 μm to about 4.6 μm. Raman Accessory from TA Instruments Iridium. These materials are selected for their inert chemistry and ease of cleaning. The choice of different interfacial unique capability enables the characterization of
especially suspensions and emulsions. microscopy. (Patent # 7,­­­­500,385) integrates with the iXR Raman rheology options gives you the greatest flexibility in choosing the appropriate geometry for your application. the interfacial response to a modified subphase
Spectrometer TM
from Thermo Fisher (Patent # 7,926,326) composition, opening possibilities for quantifying the
Scientific TM
to provide a turnkey, safe effects of changes in pH, salt, or drug concentration, or
system with Class 1 laser certification. the introduction of new proteins, surfactants, or other
active ingredients.

24 The Discovery Hybrid Rheometer 25


DHR ACCESSORIES

hree Pla e Balls on Pla


ll o n T e
Ba tes Thr te

Tribo-Rheometry
The new Tribo-Rheometry Accessory enables
measurement of the coefficient of friction between
two solid surfaces under dry or lubricated conditions.
l on Three Ball Ring on Plate
ETC Geometry SER3 Universal
The unique self-aligning design ensures uniform solid-
Bal s
solid contact and axial force distribution under all
Accessory Kits ETC Torsion Clamp Kits Testing Platform Dielectric Analysis conditions. A modular set of standard and novel
The kits feature standard geometries The Torsion Clamp Kits offer an easy way The SER3 is a universal testing platform Dielectric analysis is a powerful geometries offers a choice of different contact profiles
configured for testing thermoplastics to test solid rectangular or cylindrical to perform extensional rheology technique that measures electrical and direct simulation of end-use conditions.
and rubber, thermosetting and other samples under shear deformation on measurements and a range of physical properties such as capacitance
curing systems, pressure-sensitive the rheometer. This type of torsional material property measurements such and conductance. It can be used
adhesives and asphalt binders. A wide testing can be used to study transition as tensile, peel, tear and friction on small to characterize polar materials such
variety of stainless steel geometries of temperatures and evaluate blend solid samples. as PVC, PVDF, PMMA, and PVA, phase
various diameters and cone angles, and compatibility in multi-component separating systems, and monitor curing
disposable plates are also available to polymeric samples. kinetics in materials such as epoxy and
fully accessorize the temperature system. urethane systems. Dielectric analysis can
measure at frequencies as high as 2MHz,
well beyond traditional mechanical
limits.

26 The Discovery Hybrid Rheometer 27


DHR ACCESSORIES

Pressure Cell High Sensitivity Pressure Cell (HSPC) Starch Pasting Cell (SPC) Building Materials Cell Torsion Immersion Cell
An optional sealed vessel for studying the effect of pressure For complete viscoelastic characterization of fluids near, or The SPC is a powerful and accurate tool for rheological The Building Materials Cell is a specially designed, The Torsion Immersion Cell allows rectangular bar-
on rheological properties or materials that volatilize under above their boiling point or under pressure, the HSPC provides characterization of the gelatinization process and final abrasion-resistant and durable concentric cylinder cup shaped samples to be clamped and characterized while
atmospheric pressure. Can be used to a pressure up 100× better torque sensitivity than conventional mechanically- properties of starch products or basic characterization of and rotor for testing samples with large particles such as immersed in a temperature-controlled fluid. The resulting
to 138 bar (2,000 psi) and to a maximum temperature sealed pressure vessels. Measure low viscosities and accurate many other highly unstable materials. concrete slurries and mixes. The paddle-type rotor, slotted change in mechanical properties, caused by swelling or
of 300 °C. G’ and G” at pressures up to 5 bar, including aqueous systems cage, and the large diameter cup promote adequate plasticizing, can be analyzed in oscillatory experiments.
at temperatures as high as 150 °C. sample mixing while preventing sample slip at both the
cup and rotor surfaces.

28 The Discovery Hybrid Rheometer 29


DHR ACCESSORIES

Generic Container UV Curing Accessories


Electro-Rheology Magneto-Rheology (MR) Immobilization Cell Holder Two Smart Swap™ accessories for rheological characterization of UV-curable materials

Allows characterization of electro- The new MR Accessory enables the The new Immobilization Cell Accessory The Generic Container Holder is a are available for the HR 10, HR 20, and HR 30. One accessory uses a light guide and

rheological fluids with a voltage up to complete characterization of magneto- permits the characterization of drying, Smart Swap™ option that can hold any reflecting mirror assembly to transfer UV radiation from an external high-pressure

4000 V in both DC and AC modes. Features rheological fluids under the influence retention, and immobilization kinetics of container with an outer diameter of up mercury light source. The second accessory uses self-contained light emitting diodes

parallel plate and concentric cylinder of a controlled field. Applied fields up paints, coatings, and slurries. Solvent is to 80 mm for characterizing materials (LED) arrays featuring primary peaks of 365 nm and 455 nm. Both systems are

geometries and a maximum temperature to 1 T and a sample temperature dewatered from the sample through a with rotors. This allows for quick off-the- compatible with optional disposable plates and temperature control up to 150 °C.

of 200 °C. Flexible programmable voltage range of -10 °C to 170 °C make the paper substrate affixed to a perforated shelf evaluation of materials, such as
profiles such as step, ramp, sine, and MR Accessory ideal for all studies of MR lower plate under controlled temperature paints and varnishes, creams, pasta
triangle wave functions as well as functions fluids and ferrofluids. and vacuum. Rheological changes in sauce, etc., without creating large
with DC offsets. the sample during this immobilization shearing from sample loading. It also
process are simultaneously quantified is an excellent platform for beakers or
through an oscillatory time sweep test jacketed beakers.
with controlled axial force.

30 The Discovery Hybrid Rheometer 31


DHR FASTTRACK SYSTEM FOR ASPHALT BINDER TESTING DHR APPLICATIONS

Dry Asphalt and Asphalt Submersion Systems


TA asphalt systems meet or exceed SHRP, ASTM, and AASHTO requirements and
include 8 and 25 mm parallel plates and sample molds. The Dry Asphalt System
combines our superior Upper Heated Plate with a unique lower stepped Peltier
Plate. Flexible cooling options include Peltier, Vortex, and water circulator cooling.
The Asphalt Submersion Cell employs the classic approach of temperature
control by fully submersing the sample in circulating water.

FastTrack Software for Asphalt Binder Testing


FastTrack is a dedicated software package for ASTM- and AASHTO-compliant
testing and grading of asphalt binders on the DHR rotational rheometers.
Thoughtfully designed with the operator in mind, FastTrack consists of an
intuitive, easy-to-use graphical interface and a full suite of tests relevant to the
rheological testing of asphalt samples. Designed from the ground up, the intuitive
interface visually guides the operator through the test procedure via a series of
context-appropriate instructions and videos. Prominent visual cues convey the
instrument’s current status at a glance.

FastTrack offers a flexible configuration that can be completely optimized to


match your testing needs. This includes testing of Original Binder, Rolling Thin
Film Oven (RTFO) and Pressure Aged Vessel (PAV) residue samples, Multiple
Step Repeated Creep (MSCR) and Large Amplitude Sweep (LAS). In addition,
the Automated Temperature Calibration and Cannon standard verification tests
make it easy to run these tests for routine calibration and audit purposes.

32 The Discovery Hybrid Rheometer 33


DHR APPLICATIONS 102

Storage Stability
1. Sedimentation
2. Leveling, sagging 101

Flow Curve for Solutions and Dispersions 3. Draining under gravity


4. Chewing and swallowing Transporting Flow Curve Predicts Suitability of an

Viscosity (mPa.s)
Mixing
The Discovery Hybrid Rheometers generate flow curves as a function of stress or strain rate. More
5. Dip coating
6. Mixing and stirring
Stirring Adhesive Coating Formulation

Log η
100 Pipe Flow
7. Pipe flow
often, a flow curve is generated based on stepped flow profile, where each data point reflects 8. Spraying and brushing Shear-thinning is an important trait, particularly in coating applications. A high viscosity at low
a steady-state measurement as determined automatically by the measurement system. The 9. Rubbing
shear rates is desirable to provide stability against settling of dispersed phases during storage.
10. Milling pigments in fluid base
data generated provides information on yield stress, viscosity, shear thinning, shear thickening, or 10-1
11. High speed coating A low viscosity is desired at low rates to facilitate mixing, stirring, and transport through pipes.
4 Formulation A
thixotropy, and correlates to processing and product performance. Simple techniques like spindle Most importantly, a low viscosity at higher rates is required to permit fast coating and a low film
5 Formulation B
Coating Application
viscometers can only measure a point or a small part of the total flow curve. The broad operating 6 8 9
thickness. For the two formulations described to the right, both provide comparable moderate
1 2 3 7 10 11 10-2

range of the Discovery Hybrid Rheometer enables a complete characterization of the flow behavior 10-5 10-4 10-3 10-2 10-1 100 101 102 103 104 105 106 10-2 10-1 100 101 102 102 rate viscosity, but formulation A exhibits more desirable viscous behavior for both storage stability
of a material. Shear Rate (s-1) Shear Rate (1/s)
and coating performance.

106 106
Reference Temperature = 210 ˚C
Extended Frequency Range with TTS
Flow Curve for Polymers
A polymer’s molecular weight greatly influences its zero-shear viscosity, while its molecular weight
First Newtonian Plateau
η0 = Zero Shear Viscosity
Power Law Region 105 105
Viscoelastic Mastercurve
η0 = K • MW3.4
distribution and degree of branching affect its shear rate dependence. These differences are most Extend Range
104 104
The adjacent figure illustrates a viscoelastic fingerprint for a linear homopolymer and the variation
with Time

G’ (Pa)

G”(Pa)
Temperature of G’ and G” as a function of frequency. As frequency is the inverse of time, the curve shows the
apparent at low shear rates not possible with melt flow index or capillary devices. In addition to

Log η
Superposition
(TTS)
basic information about flow behavior, this data can be used by the powerful TROS software to & Cox-Merz 103
time-dependent mechanical response, with short times (high frequency) corresponding to solid-
103
determine molecular weight based on the measured zero shear viscosity. Cox-Merz and TTS can like behavior and long times (low frequency) to liquid–like behavior. The magnitude and shape of
1. Molecular Structure Extend
Second
be used to extend the data to higher shear rates by combining this data with data from oscillatory 2. Compression Molding Range
Newtonian
the G’ and G” curves depend on the molecular structure. Frequency sweeps are typically run over
3. Extrusion with 102 Experimental 102
Oscillation Plateau
measurements. 4. Blow and Injection Molding
& Cox-Merz
Frequency Range a limited range of 0.1 to 100 rad/s. Time-temperature superposition (TTS) is often used to extend the

1 4
frequency range by combining measurements made at several temperatures.
2 3 101 101
10-5 10-4 10-3 10-2 10-1 100 101 102 103 104 105 106 0.010 0.10 1.00 10.0 100.0 1000 10000 1.0E5
Shear Rate (s-1) ω (rad/s)

Creep and Recovery


10000
Data from creep and recovery experiments performed on paint samples that were reported to 50 Beginning of Structure Breakdown
Creep step: Stress > 0
have “good” and “bad” performance are shown in the figure to the right. This testing mode is a
Strain Sweeps Predict Dispersion Stability
powerful tool for measuring viscoelastic properties and understanding and predicting material 40 Recovery step: Stress = 0
Linear Region The accompanying figure contains the results of an oscillation strain sweep used to determine
performance when under loads for long periods of time. Examples include settling stability in Low η
1000
(unbroken Structure)
the linear viscoelastic region (LVR) and to investigate dispersion stability. In the LVR, the material

G' (Pa)
complex fluids, and zero shear viscosity (η0) and equilibrium recoverable compliance (Je0) in 30

Strain (%)
polymer melts. Creep is an especially accurate and sensitive method for determining η0 and responds linearly to the stress or strain (elastic) and the structure remains unchanged. The rapid
very low levels of elasticity; it is best-suited for the unmatched stress-control and low inertia of the 20
High η Bad Structure Breakdown drop of the modulus with strain represents breakdown of the material’s structure. Once the structure
100
Discovery Hybrid Rheometer. A similar experiment, stress relaxation, may also be performed in which has been disrupted, G’ becomes dependent on the applied strain. A material with a large linear
Good Poor Stability region is often found to be more resistant to phase separation or agglomeration.
a step strain is applied, and stress is measured as a function of time. This experiment provides a 10
Good Stability
stress relaxation modulus G(t).
10
0
0 300 600 900 1200 0.01 0.1 1 10
Time (s) Oscillation Strain (%)

34 The Discovery Hybrid Rheometer 35


DHR APPLICATIONS DHR STRONGER INSIGHTS FROM BETTER MEASUREMENTS
103
102

Yield Stress: 0.029 Pa


Determination of a Weak Yield Stress in a Suspension
Viscoelastic Structure Development Initial G’
Complex fluids often employ an engineered yield stress to support a suspended phase from settling or agglomerating,

Storage Modulous (Pa)


Recoverable G’

Loss Modulous (Pa)

Viscosity (cP)
The elastic structure of a dispersion is helpful to hold shape or stabilize dispersed particles. It is often 10 2 or to prevent a liquid from spreading at rest. This stress must be optimized such that it is large enough to prevent
desirable that this structure be broken down easily under large deformations to facilitate transport settling, but minimized so start-up of macroscopic flow is not hindered. The example data to the left shows the
or spreading, as in an architectural coating or paint. Once the deformation stops, the quiescent behavior of a beverage that suspends a dispersed phase. The yield stress and the post-yield viscosity must be low
structure should recover quickly enough to stabilize the dispersion and prevent dripping, but slowly to allow easy pourability and acceptable sensory perception when drunk. The extremely sensitive measurement of
enough to allow relaxation or smoothing of brush streaks. The time-based measurement of G’ and the HR 30 allows for this very low yield stress (0.03 Pa) to be measured readily, and with ample data before the yield
G” allows for this process to be quantified and ensure that it occurs within a target window of time to clearly establish a pre-yield plateau.
101
γ0=0.1% γ0=100% γ0=0.1% 10-3 10-2 10-1 100 101
profiles. ​ 101

0 100 200 300 400 500 600 Stress (Pa)


Time (s)

107 103
Extensional Viscosity Measurements Single Reader
G’ and G” through cure improved by Optical Encoder Dual Reader

Loss Modulus (Pa)


10 6 LDPE 1810H 10 6
Dual Reader
T=150˚C 102
The Discovery Hybrid Rheometer can also perform extensional viscosity measurements of polymers 105 A thermoset resin may undergo a dramatic change in rheological properties as it moves through the curing process.

Extensional Viscosity (Pa.s)


melts when paired with the EVA (Extensional Viscosity Accessory) or SER3 (Sentmanat Extension
104 101 The material begins as a low-viscosity liquid and converts into a high-stiffness solid in a short period of time. It is,
Rheometer). Extensional viscosity measurements are shown for standard LDPE 1810H at 150 ˚C at​
therefore, incumbent on the rheometer to make an accurate measurement over the full range of material properties

Tan (delta)
105
10 3

extensional rates from 0.02 to 3 s-1.These results are compared to three times the corresponding low 3x shear viscosity 100 with a single experimental set-up. The Optical Encoder Dual Reader improves phase angle, δ, and therefore G’ and
102
shear rate viscosity, which agrees well with the zero-rate extensional viscosity prior to the onset of

Storage Modulus (Pa)


Elongation rate (s-1) G” accuracy under all measurement conditions.This can be readily seen in the example data to the left. A rheometer
extensional thickening at different extension rates. In addition to extensional viscosity, these devices 101 10-1
104 0.02 with a conventional single reader has difficulty accurately measuring G’ before the cure or G” after the cure.
can also be used for solids tensile testing, tear testing, peel testing, as well as high-rate fracture 0.1 100
0.3 The HR 30 with Optical Encoder Dual Reader produces superior data in both cases.
10-2
testing, providing a natural complement to shear rheology that enhances material insights. ​ 1.0
10-1
3.0

103 10-2 10-3


0.01 0.1 1 10 100 1000 0 500 1000 1500 2000 2500 3000

Time (s) Time (s)

Coefficient of Friction Measurement​


104
The accompanying figure shows the coefficient of friction profiles of two commercial toothpastes. Gel Toothpaste 2.0 103 800 102 Advanced Technology for Superior Sensitivity
1.1 Whitening Toothpaste
The whitening toothpaste, with abrasive particles, has higher friction at low speeds, but the gel Exceptional torque accuracy and sensitivity enables measurements of lower viscosities,
1.0

Complex Viscocity (mPa.s)


103
toothpaste’s friction profile shows a rapid increase at higher speeds.This behavior can be explained 1.5 102 600 weaker intermolecular forces, and lower sample volumes. The low friction magnetic thrust
0.9

Viscocity (mPa.s)
Coefficient of Friction
by comparing the flow curves of the two toothpastes – although both materials are shear thinning,

Viscosity (Pa.s)
101 bearing and high accuracy Advanced Drag Cup Motor allows the Discovery Hybrid

Torque (nN.m)

Torque (nN.m)
0.8
the viscosity of whitening toothpaste decreases more rapidly than the gel toothpaste. This results Rheometer to achieve superior measurement sensitivity in both flow and oscillation
102 1.0 101 400
in increased hydrodynamic drag and greater friction at higher rotation speeds. Measurement of 0.7
conditions. This enables scientists to learn more about a material, while consuming less.
0.932 nN.m 0.252 nN.m
coefficient of friction is one of the many complementary measurements beyond shear rheology 0.6 100 One simple demonstration of this performance is the measurement of a Newtonian oil.
0.5 100 200
that are possible with the Discovery Hybrid Rheometer.​ 0.5
101 These materials exhibit a constant viscosity at all shear rates, amplitudes, or frequencies.
0.4 Simple measurements demonstrate that the HR 30 achieves sensitivity to 1 nN.m, and 0.3
0.0 10-1 0 10-1 nN.m or better in flow and oscillation testing conditions, respectively.
0.3 100 10-2 10-1 100 101 10-4 10-3 10-2 10-1
0 10-2 10-1 100 101 Shear Rate (s-1) Strain (%)
Velocity (rad/s)

36 The Discovery Hybrid Rheometer 37


DHR SPECIFICATIONS

Technical Specifications DMA Mode Instrument Features


Specification HR 30 HR 20 HR 10 Specifications Features HR 30 HR 20 HR 10

Bearing Type, Thrust Magnetic Magnetic Magnetic Motor Control Force Rebalance Transducer Optical Encoder Dual Reader ­—
Bearing Type, Radial Porous Carbon Porous Carbon Porous Carbon Minimum Force in Oscillation 3 mN DMA Mode ­—
Motor Design Drag Cup Drag Cup Drag Cup Maximum Axial Force 50 N True Position Sensor (TPS)
Minimum Displacement
Minimum Torque (nN.m) Oscillation 0.3 1 5 0.01 μm Controlled stress (steady, transient, oscillation)
in Oscillation
Minimum Torque (nN.m) Steady Shear 1 3 5 Controlled strain (steady, transient, iterative oscillation)
Maximum Displacement
Maximum Torque (mN.m) 200 200 200 100 μm Direct Strain (oscillation)
in Oscillation
Torque Resolution (nN.m) 0.05 0.1 0.1 Fast data collection ­—
Axial Frequency Range 6×10-5 rad/s to 100 rad/s
Minimum Frequency (Hz) 1.0E-7 1.0E-7 1.0E-7 Normal Force measurements with FRT
(10-5 Hz to 16 Hz)
Maximum Frequency (Hz) 100 100 100 Axial and tack testing
Minimum Angular Velocity[1] (rad/s) 0 0 0 One-Touch-Away™ Display
Maximum Angular Velocity (rad/s) 300 300 300 Integrated Sample Lighting
Displacement Transducer Optical Encoder Optical Encoder Optical Encoder FastTrack
Optical Encoder Dual Reader Standard Standard N/A AutoPilot
Displacement Resolution (nrad) 2 2 10
Step Time, Strain [2]
(ms) 15 15 15 Included Optional ­— Not Available
Step Time, Rate [2]
(ms) 5 5 5­­­
Normal/Axial Force Transducer FRT FRT FRT
Maximum Normal Force (N) 50 50 50
Normal Force Sensitivity (N) 0.005 0.005 0.01
Normal Force Resolution (mN) 0.5 0.5 1

[1] Zero in controlled stress mode. Controlled rate mode depends on duration of point being measured and sampling time.
[2] Results at 99% of commanded value

38 The Discovery Hybrid Rheometer 39


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©2020 TA Instruments/Waters Corporation. Printed in the U.S.A. March 2020 L50028.001 www.tainstruments.com www.waters.com

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