2013TA DHRGettingStartedGuide
2013TA DHRGettingStartedGuide
(DHR Series)
The material contained in this manual, and in the online help for the software used to support this instru-
ment, is believed adequate for the intended use of the instrument. If the instrument or procedures are used
for purposes other than those specified herein, confirmation of their suitability must be obtained from TA
Instruments. Otherwise, TA Instruments does not guarantee any results and assumes no obligation or liabil-
ity. TA Instruments also reserves the right to revise this document and to make changes without notice.
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erty covering subject matter in this document. Except as expressly provided in written license agreement
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marks, copyrights, or other intellectual property.
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a license to use these software programs on the module and controller with which they were purchased.
These programs may not be duplicated by the purchaser without the prior written consent of TA Instru-
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licenses are granted to the purchaser other than as specified above.
©2013 by
TA Instruments — Waters LLC
159 Lukens Drive
New Castle, DE 19720
Please click the TA Manual Supplement link to access the following important information
supplemental to this Getting Started Guide:
• TA Instruments Trademarks
• TA Instruments Patents
• Other Trademarks
• TA Instruments End-User License Agreement
• TA Instruments Offices
This manual uses NOTES, CAUTIONS, and WARNINGS to emphasize important and critical
instructions.
CAUTION: A CAUTION emphasizes a procedure that may damage equipment or cause loss of data if not fol-
lowed correctly.
Regulatory Compliance
Safety Standards
For Canada
CAN/CSA-C22.2 No. 61010-1 Safety requirements for electrical equipment for measurement, control, and
laboratory use, Part 1: General Requirements.
CAN/CSA-C22.2 No. 61010-2-010 Particular requirements for laboratory equipment for the heating of
materials.
For European Economic Area
(In accordance with Council Directive 2006/95/EC of 12 December 2006 on the harmonization of the laws
of Member States relating to electrical equipment designed for use within certain voltage limits.)
EN 61010-1:2001 Safety requirements for electrical equipment for measurement, control, and laboratory
use, Part 1: General Requirements + Amendments.
EN 61010-2-010:2003 Particular requirements for laboratory equipment for the heating of materials +
Amendments.
For United States
UL61010-1:2004 Electrical Equipment for Laboratory Use; Part 1: General Requirements.
UL61010A-2-010:2002 Particular requirements for laboratory equipment for the heating of materials +
Amendments.
Required Equipment
While operating this instrument, you must wear eye protection that either meets or exceeds ANSI Z87.1
standards. Additionally, wear protective clothing that has been approved for protection against the
materials under test and the test temperatures.
Instrument Symbols
The following label is displayed on the instrument for your protection:
Symbol Explanation
This symbol on the DHR indicates that you should read this Getting Started
Guide for important safety information. This guide contains important warnings
and cautions related to the installation, operation, and safety of the instrument.
This symbol indicates that a hot surface may be present. Take care not to touch
this area or allow any material that may melt or burn to come in contact with
this hot surface.
This symbol indicates that you are advised to consult this manual for
instructions.
Please heed the warning labels and take the necessary precautions when dealing with these areas. This
Getting Started Guide contains cautions and warnings that must be followed for your own safety.
WARNING: The material used on the top surface of the Peltier Plate is hard,
chrome-plated copper and the material used for the 'skirt' of the Peltier is stain-
less steel. Therefore, use an appropriate cleaning material when cleaning the
Peltier Plate.
WARNING: The internal components of the ETC are all constructed from chemi-
cally resistant materials, and can therefore be cleaned with standard laboratory
solvents. The only exception is the cladding for the thermocouples, which
should not be immersed in a solvent for long periods. Use a small amount of
solvent on a soft cloth and wipe the soiled area gently. This procedure should
never be conducted at any temperature other than ambient.
WARNING: The various surfaces and pipes of the ETC and the supply Dewar can
get cold during use. These cold surfaces cause condensation and, in some
cases, frost to build up. This condensation may drip to the floor. Provisions to
keep the floor dry should be made. If any moisture does drip to the floor, be sure
to clean it up promptly to prevent a slipping hazard.
WARNING: The Starch Pasting Cell (SPC) impeller is constructed from a rigid
polymer composite material of density about 1.6 g cm-3. The usual operating
angular speed is 160 rpm (16.76 radians per second). Under these conditions
the unit is unlikely to provide a significant hazard to the user, and only the
normal precautions observed when operating the rheometer need be taken.
The instrument software does permit operation of the rheometer at its maximum
angular speed, without immersion of the impeller. Take reasonable precautions
to avoid contact with the impeller when it is rotating at high angular speed.
Ensure that clothing, jewelry, etc. does not become entangled in the impeller.
Electrical Safety
Always unplug the instrument before performing any maintenance.
Supply voltage: 110 to 230 VAC
Fuse type: 2 x T15A H250 V
Mains frequency: 50 to 60 Hz
Power: 1.4 kW
Potential Asphyxiant
WARNING: Liquid nitrogen can cause rapid suffocation without warning.
Store and use in an area with adequate ventilation. Do not vent liquid nitrogen
in confined spaces. Do not enter confined spaces where high concentrations
of nitrogen gas may be present unless the area is well ventilated. The warning
above applies to the use of liquid nitrogen. Oxygen depletion sensors are
sometimes utilized where liquid nitrogen is in use.
Extremes of temperature
During operation, extreme hot or cold surfaces may be exposed. Take
adequate precautions.
Wear safety gloves before removing hot or cold geometries.
Chemical Safety
• Do not use hydrogen or any other explosive gas with the ETC.
• Use of chlorine gas will damage the instrument.
• If you are using samples that may emit harmful gases, vent the gasses by placing the instrument
near an exhaust.
WARNING: The cover should only be removed by authorized personnel. Once the
cover has been removed, live parts are accessible. Both live and neutral supplies
are fused and therefore a failure of a single fuse could still leave some parts live.
The instrument contains capacitors that may remain charged even after being dis-
connected from the supply.
WARNING: Use two people to lift and/or carry the instrument. The instrument is
too heavy for one person to handle safely. Refer to Figure 26 for lift handle loca-
tions.
Index ................................................................................................................................................... 54
Overview
This chapter reviews the history of rheology, and traces the development of combined motor and trans-
ducer (CMT) rheometers. The three models in the Discovery Series are introduced, and brief descriptions
of their main components and accessories are given. Please read this chapter carefully to familiarize
yourself with the terminology used throughout this manual.
Figure 2 CSR.
Figure 3 CSL2.
Figure 4 AR-G2.
Head
Draw rod
Column
Coolant connections
Front panel
Description
The body of the rheometer is a rigid, single-piece metal casting comprising a base and column.
The instrument head is attached to a ball-slide, which is mounted within the column. The vertical position
of the head is controlled by driving the screw of the ball-slide. The head contains the following:
• The drag cup motor, with an armature that forms the rotating spindle of the rheometer.
• A magnetic thrust bearing that supports the drive shaft and two radial air bearings that align it.
• An optical encoder that determines its angular position.
Each of these components is described in more detail in “Key Rheometer Components” on page 19.
Casting
The body of the rheometer is a single-piece aluminium casting, consisting of a base and column. The cast-
ing is an important component of the rheometer, as it needs to be rigid to axial and torsional stresses,
robust, and capable of being machined to high precision and accuracy to ensure correct alignment of the
other components of the instrument. Computer Numerical Control (CNC) machining is used to ensure con-
centricity, flatness and parallelism in the measuring system when attached.
Ball Slide
The instrument head assembly containing the motor, bearing, and optical encoder is mounted on a stiff,
linear motion, precision ball slide guide. The ball slide is mounted within the instrument column. A motor
located in the base of the casting drives the ball slide screw, moving the instrument head vertically. Its posi-
tion is measured by a linear encoder mounted on the ball slide.
Encoder
Thrust bearing
Radial bearings
Drag cup
Motor
The requirement that the bearing used on the rheometer should be low in friction applies equally to the
motor. The Discovery Series rheometers use a non-contact “drag cup” motor. A thin-walled metal cup is
mounted on the rotating spindle of the rheometer. A magnetic field rotating at thousands of revolutions per
minute is generated by continuously varying the current supplied to stationary pole pieces surrounding the
cup. This produces an eddy current in the cup, which generates a second magnetic field. The two fields
oppose each other, in accordance with Lenz's law, and the cup field is forced to follow the rotating field.
Hence, the cup is “dragged” round by the rotating field, and a torque is generated whether the cup moves or
not.
Drag cup motors have many desirable characteristics besides their low friction. Since they have no fixed
magnets, the torque produced is independent of the angular position. Futhermore, the torque is approxi-
mately proportional to the square of the current, which means that a wide torque range is produced by a rel-
atively narrow current range. The rotating components of the motor have a very low moment of inertia—
the limit is the thinness to which the cup walls can be machined. Low inertia is important whenever the
angular velocity of the moving parts is changed, for example, during transient or dynamic experiments, or
steady changes in torque.
Drag cup motors can get hot during use, and the torque output will vary with temperature. The motor
incorporates a patented drag cup temperature sensor. The temperature of the drag cup is measured, and the
input to the motor corrected, ensuring the most accurate possible torque output.
The low friction and inertia of the motor, together with sophisticated modern electronics allow close con-
trol of the motor, both in its native, controlled torque mode, and through feedback in controlled displace-
ment or angular velocity mode. Although designed according to the principles of traditional controlled-
stress rheometers, the Discovery Series rheometers are better regarded as both controlled-stress and
controlled-strain rheometers.
Optical Encoder
The transducer used to determine the angular position of the rotating spindle should have high resolution,
low friction (i.e., non-contact), low moment of inertia, and a rapid linear response. These criteria are met
by an optical encoder. This consists of a non-contacting light source and photocell, arranged on either side
of a transparent disc mounted on the rheometer spindle. At the edge of this disc are extremely fine, photo-
graphically etched radial lines, which form a diffraction grating. A stationary segment of a similar disc is
also mounted between the light source and the photocell, and the diffraction pattern formed by the light
transmitted through the gratings is detected by the photocell. As the spindle rotates, the diffraction pattern
changes. The associated electronic circuitry interpolates and digitizes the resulting signal, to produce digi-
tal high resolution, angular position data.
The angular velocity of the rotating spindle is calculated from successive readings of the angular position,
and since this is done at electronic processor speed, the encoder effectively has two outputs, the angular
position and the angular velocity.
In the DHR-3, the performance of the encoder is enhanced by using a dual reader configuration. This pat-
ent pending design improves the basic resolution and noise level of the displacement signal as well as
removing drift and improving phase resolution.
Front Panel
Some of the operation of the rheometers can be controlled through buttons on the front panel (shown in the
figure below), as well as through the instrument control software (TRIOS Software).
Smart Swap™
The Discovery Series rheometers feature “Smart Swap” technology that automatically senses the tempera-
ture control system present and configures the rheometer operating software accordingly, loading all rele-
vant calibration data. The use of this feature is covered in this manual.
Also standard across the entire range are Smart Swap™ geometries. These geometries can be automati-
cally identified when installed on the rheometer. The magnetic coating on the head of each geometry pro-
vides the read/write technology that will uniquely identify it to the instrument.
Peltier Plate
The standard Peltier Plate is the most widely-used temperature control system for the rheometers. It uses
the Peltier thermoelectric effect to control the temperature accurately, with rapid heating and cooling. The
plate consists of a copper disc, with hard chrome plating on the upper surface. A Pt100 temperature probe
is embedded in the disc, in thermal contact with it and close to the surface. Copper is used as the disc mate-
rial for its very high thermal conductivity, ensuring negligible temperature gradients across the surface of
the plate. The hard chrome plating prevents mechanical or chemical damage to the plate.
The Dual Stage Peltier Plate (DSPP) is a system optimized for low temperature measurements using the
standard four element array as a heat sink for a single Peltier element and top plate. This still has the same
maximum temperature as the standard plate, but because the lower Peltier elements are the heat sink for the
top element rather than a circulating fluid, low temperatures can be reached quickly, and without the use of
expensive refrigerated fluid circulators.
Refer to the Peltier Plate Getting Started Guide for additional information.
Geometry
holder Trough
Glass window
Check valve
DWR geometry
Du Noüy Ring
üy Ring
Interface
Dish Fluid
The Pressure Cell is a sealed vessel that can be pressurized up to 138 bar (2000 PSI) over a temperature
range of –10 to 150°C. It can be used either in self-pressurizing mode, in which the pressure is produced by
the volatility of the sample, or by externally applying the pressurization, typically with a high pressure tank
of nitrogen gas. All necessary plumbing and gauges are included as a manifold assembly. The Pressure
Cell is ideal for studying the effect of pressure on rheological properties, as well as studying the materials
that volatilize under atmospheric pressure. This option is available for all Discovery Series Rheometers.
Refer to the Pressure Cell Getting Started Guide for additional information.
WARNING: After ETC use, do not turn off the cooling air to the ETC Viewer
until the unit has returned to room temperature. Doing so could damage the
lens assembly and/or camera chip.
The ETC (Environmental Testing Chamber) Viewer is as an option that can be used with the rheometer for
the following purposes:
• Viewing the edge of plates and cones and the torsion sample
• Capturing images with data point (not fast sampling)
• Viewing point image in TRIOS results files
The viewer assembly is air cooled to allow it to perform over the whole temperature range of the ETC (-
160 to 600°C). The primary and secondary illumination, as well as the focusing aspects of the viewer, are
all controlled from within TRIOS Software.
Refer to Figure 14 for an image of the ETC Viewer.
Sleeve with
magnetic strip
Geometry base
Item/Area Specifications
Main Instrument
Width 32 cm (12.5 in)
Height 76 cm (30 in)
Depth 42 cm (16.5 in)
Weight 32 kg (70.5 lbs)
Electronics Box
Width 26 cm (10 in)
Height 48 cm (19 in)
Depth 44 cm (17 in)
Weight 14 kg (31 lbs)
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.
Item/Area Specifications
Main Instrument
Width 32 cm (12.5 in)
Height 76 cm (30 in)
Depth 42 cm (16.5 in)
Weight 32 kg (70.5 lbs)
Electronics Box
Width 26 cm (10 in)
Height 48 cm (19 in)
Depth 44 cm (17 in)
Weight 14 kg (31 lbs)
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.
Item/Area Specifications
Main Instrument
Width 32 cm (12.5 in)
Height 76 cm (30 in)
Depth 42 cm (16.5 in)
Weight 32 kg (70.5 lbs)
Electronics Box
Width 26 cm (10 in)
Height 48 cm (19 in)
Depth 44 cm (17 in)
Weight 14 kg (31 lbs)
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.
Overview
Normally the installation of your new system will be carried out by a member of the TA Instruments sales
or service staff, or their appointed agents, and it will be ready for you to use. However, should you need to
install or relocate the instrument, this chapter provides the necessary instructions.
In
• An indoor area only (A clean environment).
• Altitude up to 2000 m.
• A temperature-controlled area (5°C to 40°C).
• An area where the maximum relative humidity is 80% for temperatures up to 31°C, decreasing linearly
to 50% relative humidity at 40°C.
• An area with ample working and ventilation space around the instrument, approximately 2 meters in
length, with sufficient depth for a computer and its keyboard.
On
• A stable, vibration-free work surface.
Near
• A power outlet. (Mains supply voltage fluctuations not to exceed ±10% of the nominal voltage, instal-
lation category II.)
• Your computer for direct connection of a Serial or network port.
• Air Bearing Gas Pressure (air or nitrogen) must be clean, dry, oil-free compressed gas at 345–690 kPa
gauge (50–100 psig). The dew point should be –20°C or better. Flow rate should be 25 L/min. A 1/4
NPT female connection must be provided for the rheometer main gas supply.
Away from
• Dusty environment (pollution degree 2).
• Exposure to direct sunlight.
• Poorly ventilated areas.
After you have decided on the location for your instrument, refer to the following sections to unpack and
install your Discovery Series rheometer.
Signal port
Power port
AIR IN connection
Supply/Return
connections for
Peltier
Supply/Return
connections for
motor cooling
Power port
AC power socket
AC power switch
4 Rotate the draw rod clockwise. The draw rod screw thread will pull the geometry upwards into position
on the spindle. It should be screwed finger tight, but not forced.
NOTE: If Smart Swap is turned on, the geometry rotates a few seconds after it is fitted to enable
identification.
NOTE: To remove the geometry, perform this operation in reverse.
Figure 22 Aligning the Smart Swap geometry notch and Smart Swap cover notch.
2 Press and hold down the cycle display button (do not lift your finger off the button). The display will
cycle to the TA Logo view, and gradually the display will brighten. Release the button when the display
brightness is sufficient.
WARNING: The cover should only be removed by authorized personnel. Once the
cover has been removed, live parts are accessible. Both live and neutral supplies
are fused and therefore a failure of a single fuse could still leave some parts live.
The instrument contains capacitors that may remain charged even after being dis-
connected from the supply.
WARNING: Use two people to lift and/or carry the instrument. The instrument is
too heavy for one person to handle safely. Refer to Figure 26 below for lift handle
locations.
3 Lifting the instrument should always be done with two people. With each person standing on either side
of the instrument, place hands in the locations shown below and lift upwards, keeping the instrument in
an upright position. See the figure on the next page.
4 Treat the rheometer with the same degree of care you would take with any scientific laboratory instrument.
System Issues
Module name Firmware status Module status Module POST
Firmware status can be: Not found, Unknown, Outdated, Current, Newer, Experimental
8 Sensor fault
10 Output fault
80 CAN rx overflow
A
Asphalt Submersion Cell
description 28
auto gap set facility 23
axial force transducer 22
B
ball slide 19
C
casting 19
E
electrical safety 8
Electrically Heated Plate
description 27
ETC
description 29
ETC Viewer 33
F
front panel 22
G
geometry 45
I
installation 39
connecting the system 41
geometry 45
location requirements 40
instrument
components 19
L
LCD display
adjusting brightness 48
location of instrument 40
M
magnetically-levitated bearing 20
motor 21
O
optical encoder 21
P
Peltier Concentric Cylinder
description 25
Peltier Plate
description 24
Pressure Cell
description 32
S
safety 6
chemical 9
electrical 8
instrument symbols 6
liquid nitrogen 9
Safety Standards 4
SALS Accessory
description 33, 34
Smart Swap 23
T
True Position Sensor 23
U
unpacking 39
Upper Heated Plate
description 26
UV Curing Accessory
description 33
W
Warnings 7