Quick Start e-Training Course Discovery Hybrid Rheometer (DHR)
Thank You!
Thank you for being a TA customer This is a course designed for new users of the Discovery Hybrid Rheometer (DHR) and TRIOS software for instrument control and analysis. If the DHR has not already been installed, please refer to the DHR Getting Started Guide and/or contact a TA Instruments Service Representative before proceeding.
Course Agenda
Basic Introduction to DHR
Set up and Operation
Introduction to TRIOS software
Setting up DHR for an Experiment
Running an Experiment
Oscillation – Oscillation – Frequency Frequency Sweep
Flow – Flow – Ramp Ramp
Viewing and Presenting Data in TRIOS
What does a Rheometer do?
A Rheometer is an instrument that can measure both viscosity and viscoelasticity of a wide range of materials including: fluids, semi-solids and solids
Viscosity is defined as a material’s resistance to deformation
Viscoelasticity is a property of a material that exhibits both viscous and elastic character
A Rheometer works by relating a materials property from how hard it’s being pushed, to how far it moves
by commanding torque (stress) and measuring angular displacement (strain)
by commanding angular displacement (strain) and measuring torque (stress)
Introduction to DHR
Discovery Hybrid Rheometer (DHR) There are 3 different DHR models, all with very similar physical appearance, but with different specifications.
HR-1
HR-3
HR-2
For reference, locate the model number on the front name plate as shown here.
DHR Instrument
Electronics Box
DHR Instrument
Electronics Box
Capacitive Touch Keypad
DHR Instrument
Electronics Box
Color Display
Capacitive Touch Keypad
DHR Instrument
Electronics Box
Color Display
Smart Swap Geometry (Upper geometry)
Smart Swap Temperature System (Lower geometry) Capacitive Touch Keypad
DHR Set Up and Operation
DHR and Accessory Getting Started Guides
List of ‘Getting Started’ guides from the desktop icon
Instrument Start Up Procedure
A
Air on (30 psi)
C
Remove Cap
P
Power up DHR
Instrument Start Up Procedure – Step 1
A
Make sure that Air is connected at 30 psi to DHR Gas inlet
DHR rear panel
30 psi (2.07 bar)
Instrument Start Up Procedure – Step 2
C
Remove black Cap (bearing lock)
Twist draw rod (counter-clockwise)
and Hold cap
Instrument Start Up Procedure – Step 3
P
Turn the Power on
Off
On
On/Off switch is located on the back panel of the electronics box
Is the DHR Ready to Use?
When the DHR has been powered up correctly and is ready to use, the display status should read ‘Idle’ and the keypad should have a green and red light on the start and stop buttons
Introduction to TRIOS Software
Open TRIOS Software and Connect to DHR
Open TRIOS software
Version 3.2 or higher
Download from www.tainstruments.com
Connect to DHR
Introduction to TRIOS
TRIOS Help Menu
Browse the contents list or search using the search tab Access to Getting Started Guides also found through the help menu
TRIOS Basics – Experiments
TRIOS Basics – Results
TRIOS Basics – Results
TRIOS Basics – Geometries
TRIOS Basics – Calibration
TRIOS Basics – Control Panel
Setting up for an Experiment
Basic Steps for Experimental Set Up
1. Select a temperature control system and install 2. Select a geometry, install and equilibrate temperature a) Zero the geometry gap at the measurement temperature b) Calibrate and map the geometry (if necessary)
3. Set up the experimental parameters 4. Load and trim the sample, then start the experiment
DHR: Temperature Control Systems
Peltier Plate -40 to 200 C
Concentric Cylinder -20 to 150 C
Environmental Test Chamber (ETC) -160 to 600 C Upper Heated Plate (UHP) -30 to 150 C
Electrically Heated Plate (EHP) -70 to 400 C
DHR: Geometry Options
Concentric Cylinders
Cone and Plate
Parallel Plate
Very Low to Medium Viscosity
Very Low to High Viscosity
Very Low Viscosity to Soft Solids
Torsion Rectangular
Solids
Alternative Video Resources Strategies for Better Data - Rheology
Videos available at www.tainstruments.com
Basic Steps for Experimental Set Up
1. Select a temperature control system and install 2. Select a geometry, install and equilibrate temperature a) Zero the geometry gap at the measurement temperature b) Calibrate and map the geometry (if necessary)
3. Set up the experimental parameters 4. Load and trim the sample, then start the experiment
Install a Temperature Control System
Press the Smart Swap release button
Continuous green light for 10 s
Place the lower temperature control unit on the bottom stage
Install a Temperature Control System
Plug in the heat sink connections
(supply and return hoses)
Necessary for Peltier driven temperature control systems, which require fluid circulation for proper operation
Install a Temperature Control System
When using a Peltier driven device, please ensure that the external fluid circulator is always turned ON When not in use, it is strongly recommended to deactivate the Peltier device and turn off the circulator
Note: Always verify fluid levels before operation. If operating circulator below 5 C, fill the circulator with a mixture or material with a lower freezing point than water.
Install a Temperature Control System
Plug in the Smart Swap cable and verify light is off Note: if green light is blinking, press again to activate smart swap function
Green light OFF
Install a Temperature Control System
TRIOS will recognize the temperature control system Set the measurement temperature using the Environmental control panel
Set temperature and press ‘Apply’
Basic Steps for Experimental Set Up
1. Select a temperature control system and install 2. Select a geometry, install and equilibrate temperature a) Zero the geometry gap at the measurement temperature b) Calibrate and map the geometry (if necessary)
3. Set up the experimental parameters 4. Load and trim the sample, then start the experiment
Smart Swap Enabled in TRIOS
Blue check mark indicates Smart Swap is Enabled
Smart Swap Disabled in TRIOS
If Smart Swap is disabled… Manually select a geometry from the drop down list The active geometry will be indicated by a check mark
Home Position
Press and hold the electronic head lock button until an audible beep is heard The red light will blink indicating the head is locked in the home position
Install a Geometry
Align the mark on the geometry with that on the rheometer head and install onto the motor shaft
Rotate the draw rod clockwise to tighten If smart swap is enabled, TRIOS will recognize geometry installed
Raise and Lower the DHR Head
Move the upper geometry to about 5-7 mm above the lower plate
Raise/lower Head
Zero the Gap
Set initial test temperature Allow geometry time to equilibrate at temperature
Zero the geometry gap from touch pad or Gap control panel
The DHR is now ready for use
Perform a geometry calibration as desired
Running an Experiment
Basic Steps for Experimental Set Up
1. Select a temperature control system and install 2. Select a geometry, install and equilibrate temperature a) Zero the geometry gap at the measurement temperature b) Calibrate and map the geometry (if necessary)
3. Set up the experimental parameters 4. Load and trim the sample, then start the experiment
Demonstration Experiment #1
Sample:
Polydimethylsiloxane (PDMS)
Geometry:
25 mm parallel plate
Mode and Test:
Oscillation - Frequency Sweep
Temperature:
30ºC
Parameters:
1 to 100 rad/s with 5% strain
Analysis: Verify crossover modulus and frequency
TRIOS Sample Information
t n e m w i e r i e V p x E
Sample
Geometry
Procedure
TRIOS Geometry Information
t n e m w i e r i e V p x E
Sample
Geometry
Procedure
TRIOS Geometry Information
Verify appropriate geometry
Gap set to 1000 m (1.0 mm)
Set trim gap offset to 5% gap (1000 + 50 = 1050 m = Trim gap)
TRIOS Experimental Procedures
w o l F
Temperature Ramp Ramp Sweep Peak Hold
n o i t a l l i c s O
Frequency Temperature Ramp Temperature Sweep Time Amplitude Fast Sampling Manual
) t n e p i e t s S n a r T (
Creep Stress Relaxation Stress Growth Repeated Creep
TRIOS Experimental Procedure for PDMS
Basic Steps for Experimental Set Up
1. Select a temperature control system and install 2. Select a geometry, install and equilibrate temperature a) Zero the geometry gap at the measurement temperature temperature b) Calibrate and map the geometry (if necessary)
3. Set up the experimental parameters 4. Load and trim the sample, then start the experiment
Loading Sample
Set temperature and equilibrate equilibrate to 30C Zero the geometry gap at test temperature – temperature – IMPORTANT! IMPORTANT! Load sample - PDMS
Be careful - No trapped air bubbles!
Use excess material to ensure gap is filled completely
Go to Trim Gap
Go to Trim gap
From touch pad or control panel
Trim gap = Gap + Trim gap offset
Wait for axial force to relax to minimum before trimming the sample
Blinking green light indicates trim gap has reached set point
Trim the Sample
Lock the head using the electronic head lock button Trim sample edge with straight edge tool Go to geometry or measurement gap
Solid red light indicates head is locked
From touch pad or control panel
Wait for axial force to relax before starting the experiment Solid green light indicates geometry gap has reached set value
Correct Gap Filling
Start the Experiment
Start the test
Start/Stop Test
Frequency Sweep - PDMS
Frequency Sweep - PDMS
Frequency Sweep - PDMS
Demonstration Experiment #2
Sample:
Silicone Oil (1 Pa s)
Geometry:
60 mm 2 cone
Mode and Test: Flow - Ramp Temperature:
25ºC
Parameters:
0 to 88 Pa over 600 s
Analysis: Verify oil viscosity at specified temperature TA Service Representatives perform this test at installation
TRIOS Experimental Procedure for Silicone Oil
Load Silicone Oil
Set temperature to 25 C and zero the geometry gap
Load sample
Set the gap to the trim gap Lock the head and trim with nonabsorbent tool
Be careful not to introduce air bubbles!
Note: There is no need to wait for sample axial force to relax, but important to allow time for thermal equilibration
Go to geometry gap and initiate the experiment
Flow Ramp – Silicone Oil
Viewing and Presenting Data in TRIOS
Select Plot Variables
Select Plot Variables
Or with cursor over the plot area, right-click…
Axis Scaling
With cursor over the axis scale, right-click…
Create an Overlay Plot
Create an Overlay Plot
Click and drag file segments to display area
Create an Overlay Plot
Analysis Functions
Click on Analysis ribbon, select the analysis function, highlight data range to analyze and click ‘Analyze’
Analysis – Modulus Crossover
Stamp Data Point and Statistics
Stamp Data Point and Statistics
DHR Instrument Shutdown (Optional)
If there is a need to turn off the DHR For example, to conserve air or nitrogen…
P C A
Power off DHR Install Cap Air off
NOTE: Please make sure Power is OFF before installing the cap (or bearing lock). DO NOT rotate draw rod or remove cap (or bearing lock) without air supplied to the instrument.
Need DHR Assistance?
Contact the TA Instruments Rheology Applications Support line
Phone: 302-427-4167 Monday - Friday 8:00am - 4:30pm (ET)
Email:
[email protected]
Visit our Website www.tainstruments.com for training videos, TA Tech tips, application notes and much more!
