TA Instruments DHR Series User manual

Revision E Issued November 2013
Getting Started Guide
DHR Series and AR Series
Starch Pasting Cell

Page 2 DHR/AR Series Starch Pasting Cell Getting Started Guide
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.
©2013 by
TA Instruments — Waters LLC
159 Lukens Drive
New Castle, DE 19720

DHR/AR Series Starch Pasting 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

Page 4 DHR/AR Series Starch Pasting Cell Getting Started Guide
Notes, Cautions, and Warnings
This manual uses NOTES, CAUTIONS, and WARNINGS to emphasize important and critical
instructions. In the body of the manual these may be found in the shaded box on the outside of the page.
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/AR Series Starch Pasting 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/AR Series Starch Pasting Cell Getting Started Guide Page 6
Safety
Do not attempt to service this cell, as it contains no user-serviceable components.
Required Equipment
While operating this accessory, 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 accessory 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 a hot surface may be present. Take care not to touch
this area or allow any material that may melt or burn 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.

DHR/AR Series Starch Pasting Cell Getting Started Guide Page 7
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
Chapter 1:
Introducing the Starch Pasting Cell (SPC) ................................................................... 8
Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .8
System Components . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .9
Temperature Control . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .10
Chapter 2:
Installing and Setting Up the SPC System .................................................................. 11
Installing the Starch Pasting Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .11
Assembling the Starch Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .12
Attaching the Impeller . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .13
Setting the Geometry Details . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .13
Connecting the Cooling Control Unit (CCU) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .14
Setting the Cooling Water Parameters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .15
Chapter 3:
SPC Use and Maintenance ........................................................................................... 16
Running an SPC Procedure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .16
Maintaining the SPC . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .17
Bearing Friction Correction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .17
Rotational Mapping . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .17
Index ................................................................................................................................................... 18

DHR/AR Series Starch Pasting Cell Getting Started Guide Page 8
Chapter 1:
Introducing the Starch Pasting Cell (SPC)
Overview
This manual is intended as an addendum to the DHR and AR-G2/AR 2000ex/AR 1500ex Rheometer
Getting Started Guides.
The Smart Swap™ Starch Pasting Cell (SPC) is designed to measure the viscosity of starch using methods
currently in use in the starch industry.
Starch is used as a rheology modifier in many foodstuffs. As a raw material, it is normally supplied in the
form of approximately spherical granules, with diameters between about 1 µm and 100 µm. To be used as
a rheology modifier, starch must undergo gelatinization, which occurs when the granules are disrupted in
aqueous environments, to swell and eventually release the constituent molecules. The temperature at which
this process commences will depend on the nature of the starch, but it is usually approximately 60°C. The
process is thermally irreversible, and when the temperature is reduced, the system remains gelatinized,
although some slow de-gelatinization (retrogradation) may occur.
The precise gelatinization temperature, the time taken for the process to go to completion, and the rheolog-
ical properties of the gelatinized starch, will depend on the source of the starch, any physical and chemical
modifications made, the pH of the aqueous phase, and so on. Test methods have been developed in the
starch industry allowing the rapid testing of starches. The general procedure is as follows:
1Dispersal of a specified quantity of starch in water or buffer solution at low temperature
2Raising the temperature rapidly to above the gelatinization temperature
3Holding the temperature for a fixed period
4Reducing the temperature to below the gelatinization temperature
5Holding the temperature for a further fixed period
Stirring is carried out during the entire process. The stirring is necessary in the pre-gelatinization stage to
prevent the starch particles from sedimenting. In the post-gelatinization stages, it is used to ensure good
mixing.

DHR/AR Series Starch Pasting Cell Getting Started Guide Page 9
System Components
The SPC consists of four components:
•Thejacket, which is mounted on the instrument base
•Thecup, which is removable and inserts into the jacket
•Thecap, which screws onto the jacket to hold the cup in place
•Theimpeller, which attaches to the instrument spindle
These are shown in the figures below.
Figure 1 SPC properly mounted on DHR Rheometer.
Figure 2 The cup (left), cap (center), and impeller (right).
SPC jacket
Cap
Impeller

DHR/AR Series Starch Pasting Cell Getting Started Guide Page 10
Temperature Control
Heating is accomplished through the electrical elements placed within the jacket, concentrically to the cup.
The sample is cooled using water carried in a helical conduit in close proximity to the cup outer walls. The
cooling water flow is controlled through the Cooling Control Unit (CCU), which is placed upstream of the
cup.
Figure 3 Cooling Control Unit (CCU).
Purge air is used to displace the water from the conduit during heating. The temperature is read by a Pt 100
probe in close thermal contact with the cup bottom. The impeller shaft is designed to prevent significant
solvent evaporation.
NOTE: If the geometry gap is unreferenced (“unknown”) or greater than 50,000 microns, the temperature
is measured by a probe located in the jacket, rather than by the probe in contact with the cup, as it other-
wise would be.
Figure 4 Cross-section of CCU.

DHR/AR Series Starch Pasting Cell Getting Started Guide Page 11
Chapter 2:
Installing and Setting Up the SPC System
Follow the instructions in this chapter to install and set up the SPC system.
Installing the Starch Pasting Cell
Follow the instructions below to properly install the SPC on the rheometer. The SPC is a standard Smart
Swap™ accessory and is mounted/uninstalled on the rheometer as such.
1Use the Smart Swap™ connector to mount the fixture on the rheometer.
2Plug the SPC accessory cable into the rheometer accessory cable port.
Figure 5 SPC installed on DHR Rheometer.
Accessory cable

DHR/AR Series Starch Pasting Cell Getting Started Guide Page 12
Assembling the Starch Cell
Follow these instructions to assemble the SPC:
1Raise the instrument head.
2Insert the cup into the jacket, as shown below.
Figure 6 Inserting the cup into the jacket (DHR Series shown).
3Screw the cap onto the jacket, as shown below.
Figure 7 Fitting the cap onto the jacket (DHR Series shown).
CAUTION: To avoid damaging the threads, do not over tighten. The purpose of the cap is to prevent
rotation of the cup and to ensure good thermal contact between the base of the cup and the tempera-
ture sensor. Light finger tightness should be sufficient to achieve this.
MISE EN GARDE: Pour éviter d'endommager les filetages, ne serrez pas trop. Le but du bouchon
est d'empêcher la rotation de la coupelle et d'assurer un bon contact thermique entre la base de la
coupelle et le capteur de température. Un serrage léger à la main devrait suffire pour cela.
Cup
Cap

DHR/AR Series Starch Pasting Cell Getting Started Guide Page 13
Attaching the Impeller
Install the impeller on the rheometer in the same manner you would any standard geometry.
Setting the Geometry Details
For information regarding setting up the SPC geometry in TRIOS software, see TRIOS Help topic
Creating the Starch Pasting Cell Geometry in TRIOS.

DHR/AR Series Starch Pasting Cell Getting Started Guide Page 14
Connecting the Cooling Control Unit (CCU)
The flow of the cooling water and purge air is controlled through a CCU, shown below. This unit may be
free standing, or wall mounted using the clearance holes on top of the unit.
Figure 8 Cooling Control Unit (CCU).
Connect the CCU as follows:
1Connect the air supply to the GAS IN port using the 8-mm outer diameter tubing.
2Connect the water supply to the LIQUID IN port using the 6-mmouter diameter tubing. If mains water
is used as the supply, then the non-return valve (shown below) should be placed in the line upstream of
the CCU.
Important: Note the direction of flow through this valve.
Figure 9 Non-return valve (for use with mains water supply only).

DHR/AR Series Starch Pasting Cell Getting Started Guide Page 15
3Connect the GAS/LIQUID outlet port to the upper port on the Starch Cell jacket, usingthe 4-mm outer
diameter tubing with the 4-mm to 6-mm adapter provided.
4Using the 4-mm outer diameter tubing connect the lower port on the Starch Cell jacket to the drain, if
the mains water is the supply, or to the return, if a fluid circulator is used.
5Connect the EVENTBsocket on the rear of the AR Rheometer to the EVENTsocket on the CCU using
only the cable.
6Set the air flow rate to 1 L/min. Note that the reading is taken from the center of the float. To set the
flow rate, it may be necessary to raise the temperature of the Starch Cell using the instrument software
to ensure continuous flow.
Setting the Cooling Water Parameters
For optimum temperature control, set the parameters for the cooling water from within TRIOS Instrument
Control Software.
For more information, see Setting the Cooling Water Parameters for the AR Starch Pasting Cell TRIOS
Help topic.

DHR/AR Series Starch Pasting Cell Getting Started Guide Page 16
Chapter 3:
SPC Use and Maintenance
Running an SPC Procedure
Perform the following steps to load your sample, run the experiment, then remove the sample:
1Raise the instrument head to the full back off distance.
2Remove the Starch Cell cap and cup from the jacket. See Chapter 3 for information, if needed.
3Add the ingredients to the cup, and reassemble the Starch Cell.
4Send the instrument to the correct geometry gap.
5Start the procedure. Wait until the experiment is complete.
6Remove the sample by raising the instrument head to the full backoff distance.
NOTE: If the final viscosity of the sample is high, it may be necessary to release the impeller before rais-
ing the head. To do this, hold the impeller shaft firmly, and rotate the drawrod counterclockwise (anti-
clockwise).

DHR/AR Series Starch Pasting Cell Getting Started Guide Page 17
Maintaining the SPC
Bearing Friction Correction
The friction due to the rheometer air bearing is negligible except when very low viscosity samples are
used, and no correction is normally necessary when using the Starch Cell. However, if you do wish to
introduce a correction for bearing friction, the procedure is available through the instrument control soft-
ware. See TRIOS software Online Help for details.
Rotational Mapping
Rotational mapping is used on the TA Instruments' AR Series Rheometers to ensure optimal performance
for very sensitive samples. It should not normally be necessary with the Starch Cell, but may be used if
very precise data are required at low angular velocities. See TRIOS software Online Help for details.

DHR/AR Series Starch Pasting Cell Getting Started Guide Page 18
Index
C
cautions 4
CCU
connecting 14
CCU cooling water parameters 15
I
impeller
attaching 13
instrument symbols 6
L
license agreement 3
N
notes 4
P
patents 3
R
Regulatory Compliance 4
S
safety 6
instrument symbols 6
Safety Standards 4
SPC
assembling 12
components 9
installing 11
maintenance 17
overview 8

DHR/AR Series Starch Pasting Cell Getting Started Guide Page 19
running a procedure 16
setting up geometry 13
temperature control 10
starch
testing of 8
T
TA Instruments offices 3
temperature control 10
trademarks 3
W
warnings 4