TA DHR Series User manual

Revision D Issued November 2014
Getting Started Guide
DHR Series
Immobilization Cell

DHR Series Immobilization Cell Getting Started Guide Page 2
Notice
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.
TA Instruments may have patents, patent applications, trademarks, copyrights, or other intellectual prop-
erty covering subject matter in this document. Except as expressly provided in written license agreement
from TA Instruments, the furnishing of this document does not give you any license to these patents, trade-
marks, copyrights, or other intellectual property.
TA Instruments Operating Software, as well as Module, Data Analysis, and Utility Software and their asso-
ciated manuals and online help, are proprietary and copyrighted by TA Instruments. Purchasers are granted
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-
ments. Each licensed program shall remain the exclusive property of TA Instruments, and no rights or
licenses are granted to the purchaser other than as specified above.
©2014 by
TA Instruments — Waters LLC
159 Lukens Drive
New Castle, DE 19720

DHR Series Immobilization Cell Getting Started Guide Page 3
Introduction
Important: TA Instruments Manual Supplement
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

DHR Series Immobilization Cell Getting Started Guide Page 4
Notes, Cautions, and Warnings
This manual uses NOTES, CAUTIONS, and WARNINGS to emphasize important and critical
instructions.
NOTE: A NOTE highlights important information about equipment or procedures.
CAUTION: A CAUTION emphasizes a procedure that may damage equipment or cause loss of data
if not followed correctly.
MISE EN GARDE: UNE MISE EN GARDE met l'accent sur une procédure susceptible d'endom-
mager l'équipement ou de causer la perte des données si elle n'est pas correctement suivie.
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.
A WARNING indicates a procedure that may be hazardous to the operator or
to the environment if not followed correctly.
Un AVERTISSEMENT indique une procédure qui peut être dangereuse pour
l'opérateur ou l'environnement si elle n'est pas correctement suivie.

DHR Series Immobilization Cell Getting Started Guide Page 5
Electromagnetic Compatibility Standards
For Australia and New Zealand
AS/NZS CISPR11:2004 Limits and methods of measurement of electronic disturbance characteristics of
industrial, scientific and medical (ISM) radio frequency equipment.
For Canada
ICES-001 Issue 4 June 2006 Interference-Causing Equipment Standard: Industrial, Scientific, and Medical
Radio Frequency Generators.
For the European Economic Area
(In accordance with Council Directive 2004/108/EC of 15 December 2004 on the approximation of the
laws of the Member States relating to electromagnetic compatibility.)
EN61326-1:2006 Electrical equipment for measurement, control, and laboratory use-EMC requirements-
Part 1: General Requirements. Emissions: Meets Class A requirements per CISPR 11. Immunity: Per
Table 1 - Basic immunity test requirements.
For the United States
CFR Title 47 Telecommunication Chapter I Federal Communications Commission, Part 15 Radio
frequency devices (FCC regulation pertaining to radio frequency emissions).

DHR Series Immobilization Cell Getting Started Guide Page 6
Safety
Do not attempt to service this instrument, as it contains no user-serviceable components.
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:
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.
Symbol Explanation
This symbol indicates that you should read this Getting Started Guide for impor-
tant safety information. This guide contains important warnings and cautions
related to the installation, operation, and safety of the instrument.
Ce symbole indique que vous devez lire entièrement ce guide de démarrage. Ce
guide contient d'importants avertissements et mises en garde relatifs à l'installa-
tion, à l'utilisation et à la sécurité de l'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.
Ce symbole indique la présence possible d'une surface chaude. Prenez soin de
ne pas toucher cette zone ou de laisser un matériau susceptible de fondre ou de
brûler entrer en contact avec cette surface chaude.
This symbol indicates that you are advised to consult this manual for
instructions.
Ce symbole indique que nous vous recommandons de consulter ce manuel pour
les instructions.

DHR Series Immobilization Cell Getting Started Guide Page 7
Cautions and Warnings
CAUTION: The Peltier Plate may be damaged by operating the instrument without a flow of water
through the Peltier Plate. There is a Peltier overheat protection device that will activate if the device
becomes too hot.
MISE EN GARDE: La plaque Peltier peut être endommagée si l'instrument est utilisé sans
écoulement d'eau dans la plaque Peltier. Il existe un dispositif de protection contre la surchauffe qui
s'active si le dispositif devient trop chaud.
WARNING: Take adequate precautions prior to heating of materials if it can lead
to explosion, implosion or the release of toxic or flammable gasses.
AVERTISSEMENT: Prenez des mesures de précaution adéquates avant de
chauffer des matériaux, si cela peut entraîner l'explosion, l'implosion ou le
dégagement de gaz toxiques ou inflammables.

DHR Series Immobilization Cell Getting Started Guide Page 8
Table of Contents
Introduction ................................................................................................................................................. 3
Important: TA Instruments Manual Supplement ................................................................................... 3
Notes, Cautions, and Warnings.............................................................................................................. 4
Regulatory Compliance.......................................................................................................................... 4
Safety Standards .............................................................................................................................. 4
Electromagnetic Compatibility Standards.............................................................................................. 5
Safety...................................................................................................................................................... 6
Required Equipment ........................................................................................................................ 6
Instrument Symbols ......................................................................................................................... 6
Cautions and Warnings .................................................................................................................... 7
Table of Contents ........................................................................................................................................ 8
Chapter 1: Introducing the Immobilization Cell ..................................................................................... 9
Overview ....................................................................................................................................................... 9
System Specifications ................................................................................................................................. 11
Ramp Rate............................................................................................................................................ 11
Chapter 2: Installing the Immobilization Cell ....................................................................................... 12
Removing the Immobilization Cell...................................................................................................... 15
Chapter 3: Using the Immobilization Cell .............................................................................................. 16

DHR Series Immobilization Cell Getting Started Guide Page 9
Chapter 1:
Introducing the Immobilization Cell
Overview
The Immobilization Cell is a Smart Swap™ accessory that can be used to investigate the immobilization
kinetics of a coating material as its liquid component is drawn into a substrate by a vacuum. Measurements
can be performed under different conditions of temperature, gap, pressure, and rheological deformation.
In the Immobilization Cell, a disk of the substrate under test is held in place by a clamping ring. A vacuum
is created below the substrate, and any excess fluid not absorbed by the substrate is captured in a waste
flask.
Figure 1
The temperature of the perforated platform is controlled by Peltier elements in the base of the unit. These
heat or cool the specially shaped inner jacket, which transfers the temperature to the platform.
Figure 2

DHR Series Immobilization Cell Getting Started Guide Page 10
The vacuum is controlled using the event step in Trios (see on-line help) to activate a solenoid on the waste
management manifold. The manifold also includes a valve that can be used to vent the cell and waste flask
at the end of a test, or in conjunction with the gauge on your vacuum pump to meter the pressure in the cell
during a test.
Figure 3
NOTE: A vacuum pump is not supplied as part of the system.
NOTE: You should consider installing a vapour trap to protect your vacuum pump and waste management
manifold if the vapour extracted from your sample is likely to damage these components.

DHR Series Immobilization Cell Getting Started Guide Page 11
System Specifications
The tales below contains the technical specifications for the Immobilization Cell.
CAUTION: The Peltier Plate may be damaged by operating the instrument without a flow of water
through the Peltier Plate. There is a Peltier overheat protection device that will activate if the device
becomes too hot.
MISE EN GARDE: La plaque Peltier peut être endommagée si l'instrument est utilisé sans écoule-
ment d'eau dans la plaque Peltier. Il existe un dispositif de protection contre la surchauffe qui
s'active si le dispositif devient trop chaud.
Ramp Rate
The maximum sustainable ramp rate will depend on a number of factors such as the start and end tempera-
ture and the temperature/flow rate of circulation fluid. To determine the maximum sustainable heating/
cooling rate, perform the following test and analysis:
1Equilibrate to start temperature.
Perform a time sweep or peak hold test with the temperature set (if possible) to a few degrees in excess of
the end temperature. Set the time much longer than you expect; the test can be aborted when the tempera-
ture has reached a stable value.
2Plot a graph of temperature vs. time (min) and take the derivative.
Inspect the derivative curve over your temperature range of interest. The maximum sustainable rate will be
the lowest value on the derivative curve.
Table 1: Immobilization Cell Specifications
Item/Area Specifications
Temperature Range
Tap water supply
Air cooled circulator (P/N 403209.901)
Thermo Cube (P/N 403258.901) at -5°C
(80% water/20% alcohol mixture)
-10°C to 150°C
0°C to 150°C
-10°C to 150°C
Ramp Rate See section below.
Pt100 Internal Resolution 0.01°C
Vacuum Pressure difference 0–85,000 Pa1
1. Depends on capability of pump
Cell Construction Anodised Aluminum

DHR Series Immobilization Cell Getting Started Guide Page 12
Chapter 2:
Installing the Immobilization Cell
The Immobilization Cell system consists of a temperature-controlled jacket, a perforated platform and sub-
strate clamping ring. A manifold to control the vacuum and collect waste is connected to the cell. It is used
in conjunction with an upper 50mm parallel plate geometry.
To install up the Immobilization Cell, follow these steps:
1Raise the rheometer head to the top most position.
2Press the Release button on the control panel, as shown below. A continuous green light indicates that
the attachment can be fitted.
Figure 4 Control panel.
NOTE: The release state will only stay active for 10 seconds.
Control panel

DHR Series Immobilization Cell Getting Started Guide Page 13
3Fit the Immobilization Cell, ensuring it is aligned correctly.
Figure 5 Fitting the Immobilization Cell.
4Connect the power cable and fluid hoses.
Figure 6 Connecting power cable and fluid hoses.
5When the green status light turns off, the Immobilization Cell is correctly installed.
6Attach the 50 mm Parallel Plate to the motor shaft.
Alignment lug on the lower
stage should locate in the slot
on the Smart Swap base.
Power cable
Fluid hoses

DHR Series Immobilization Cell Getting Started Guide Page 14
7Connect 6 mm pipe from the vacuum port on the side of the Immobilization Cell to one of the three
inlets on the waste flask.
Figure 7 Vacuum port (left) and waste flask manifold (right).
8Connect 6 mm tubing from one of the three inlets on the waste flask to the Vent fitting.
9Connect 6 mm tubing from one of the three inlets on the waste flask to the left side of the solenoid.
10 Connect 6 mm tubing from the solenoid to your vacuum pump.
11 Connect the 4-pin event cable from Event B on the rear of the rheometer to the Event connection.
Figure 8 Cable connections on rheometer back panel.
Waste flask inlets
Vent / Metering
Event
Solenoid
connection to
vacuum pump
Signal port
Power port
Supply/Return
connections for
motor cooling
AIR IN connection
Supply/Return
connections for
Peltier

DHR Series Immobilization Cell Getting Started Guide Page 15
Removing the Immobilization Cell
1Disconnect the 6 mm tubing from the vacuum port on the Immobilization Cell.
2Press the Release button on the control panel. A flashing green light indicates that the attachment can
be unplugged. Refer to step 2 in the previous section for Release button location.
3Press the Release button again. A continuous green light indicates that you can remove the Immobilization
Cell.
4Remove the Immobilization Cell from the rheometer.

DHR Series Immobilization Cell Getting Started Guide Page 16
Chapter 3:
Using the Immobilization Cell
1Fit the perforated platform into the body of the cell aligning the slots in the platform with the peg and
screw heads on the body. Then twist the platform clockwise and clamp in place using the two thumb
screws.
2Cut a 57 mm (2.25") disk of your substrate and place on the platform.
3Insert the retaining ring and tighten using the 3 thumb screws.
4In TRIOS, set the zero gap options to Axial force and set a force that overcomes any bow in your sample.
This value can be determined by performing an axial compression test, plotting force vs. gap and picking
a force above which the gap is invarient. The maximum allowable is 30N.
5Zero the gap and raise the head to the loading position.
6Design your experiment.
• Use event step 2 to turn the vacuum on and off
• Use axial force control in compression (typically 0N+/-1N)
• An Oscillation Time Sweep is the preferred type of test step
7Load the sample.
8Turn on your vacuum pump.
9Lower the head to the measurement gap and start the test.
10 Once the test has completed use the vent valve on the waste management manifold to relieve the vacuum
in the cell so that the head can be raised.
11 Raise the head and remove the platform, substrate, and retaining ring as once piece for easy cleaning.
Figure 9
Retaining ring
Perforated platform
Cell body