Old DSC
Old DSC
INNOVATIVE ENGINEERING
TA Instruments is the recognized leader for supplying innovative
technology, investing twice the industry average in research and
development. Our new Q Series™ Thermal Analysis modules are the
industry standard. Patented innovations like Modulated DSC®, Tzero™
technology, and Hi-Res™ TGA are available only from TA.
QUALITY PRODUCTS
All thermal analyzers and rheometers are manufactured according to ISO 9001:
2000 procedures in our New Castle, DE (USA) or our Crawley, UK facilities.
Innovative flow manufacturing procedures and a motivated, highly-skilled work force
ensure high quality products with industry-leading delivery times.
TECHNICAL SUPPORT
Customers prefer TA Instruments because of our reputation for after-sales support.
Our worldwide technical support staff is the largest and most experienced in the
industry. They are accessible daily by telephone, email, or via our website. Multiple
training opportunities are available including on-site training, seminars in our
application labs around the world, and convenient web-based courses.
New Castle, DE USA - 1-302-427-4000 • Crawley, England - 44-1293-658900 • Brussels, Belgium - 32-2-706-0080
Paris, France - 33-1-30-48-94-60 • Etten-Leur, Netherlands - 31-76-508-7270 • Eschborn, Germany - 49-6196-400-600
Milano, Italy - 39-02-27421-283 • Barcelona, Spain - 34-93-600-9300 • Melbourne, Australia - 61-3-9553-0813
Stockholm, Sweden - 46-8-59-46-92-00 • Tokyo, Japan - 81-3-5479-8418 • Shanghai, China - 86-21-63621429
Bangalore, India - 91-80-28398963
W W W . TA I N S T R U M E N T S . C O M
DIFFERENTIAL SCANNING CALORIMETERS
T THAT DESCRIBE A
FIFTH-GENERATION
TA INSTRUMENTS Q SERIES™ DIFFERENTIAL SCANNING
CALORIMETER (DSC). THE Q1000, Q100, Q10,
PRODUCTS FROM THE WORLD LEADER
AND
IN
Q10P ARE
DIFFERENTIAL
DSC
TECHNOLOGY
TA Innovations
DIFFERENTIAL THERMAL ANALYSIS
HEAT FLUX DSC
PRESSURE DSC
FIRST MICROPROCESSOR CONTROLLED CALORIMETERS
FIRST AUTOMATED DSC
DUAL SAMPLE DSC
DIFFERENTIAL PHOTOCALORIMETRY
MODULATED DSC®
TZERO™ DSC TECHNOLOGY
Q1000
The Q1000 is TA Instruments’ top-of-the-line, research-grade DSC,
with unmatched performance in baseline stability, sensitivity, and
resolution. It contains Advanced Tzero™ technology, the most
powerful DSC technology commercially available. Its industry
leading features include Modulated DSC™, a 50-position intelligent
autosampler, and digital mass flow controllers. Photocalorimetry
and pressure DSC accessories are also available, making the
Q1000 the best-equipped analyzer to meet the needs of the most
demanding researcher.
Q100
The Q100 is a versatile, research-grade DSC with our patented
Tzero™ technology. With many Q1000 performance features, the
Q100 easily outperforms competitive research models. It is an
expandable module, to which MDSC®, a 50-position autosampler,
or a photocalorimeter can be added. Innovative technology,
performance, upgradability, and ease-of-use make the Q100 a
superb addition to any laboratory.
Q10
The Q10 is a cost-effective, easy-to-use, general-purpose DSC
with basic performance features equivalent to many competitive
research-grade models. It is ideal for research, teaching,
and quality control applications that require a rugged, reliable,
basic DSC.
T E C H N I C A L S P E C I F I C AT I O N S
Temperature Range (with cooling accessory) -180 to 725 ˚C -180 to 725 ˚C -180 to 725 ˚C -130 to 725 ˚C
Baseline Curvature with Tzero (-50 to 300˚C) 10 µW 10 µW Not Available Not Available
T ECHNICAL S PECIFICATIONS 5
Q1000/Q100 TECHNOLOGY
AUTO LID
The Q1000 and Q100 have a new and improved auto
lid assembly that consists of dual silver lids and a
dome-shaped heat shield. The auto lid automatically covers
and uncovers the cell as necessary. The Q10 lid
assembly is manually operated. Benefits: More accurate
measurements result from improved thermal isolation
of the cell.
Furnace
Cooling
Rods
Cooling Ring
FURNACE
The sample and reference platforms are surrounded by a high thermal conductivity, silver furnace, that
uses rugged, long-life Platinel™ windings. Purge gases are accurately and precisely metered by mass flow
controllers and uniformly heated to cell temperature, prior to introduction to the sample chamber.
Benefits: The design provides a highly uniform thermal environment for the sample and reference.
Precise temperature control algorithms deliver accurate isothermal temperatures, linear heating rates,
rapid temperature response and the ability to heat at rates up to 200 ˚C / min. The rugged heater windings
ensure long furnace life. Superior data quality results from the uniform purge gas flow.
D E S I G N F E AT U R E S AND BENEFITS 7
Q SERIES™ ACCESSORIES
AUTOSAMPLER
The patented DSC autosampler is a powerful
performance and productivity enhancer for
the Q Series™ DSC modules. It provides
reliable, unattended operation of the Q1000
or Q100 DSC, even when using the RCS or
LNCS cooling accessories. Its 50-sample,
5-reference pan carousel tray, enables
research and analytical laboratories to
analyze samples “around-the-clock.”
The sample arm controls loading and
unloading of sample and reference pans in sequential or random order. An optical sensor guides the sample
arm, ensuring precise pan placement and automatic calibration of the system. Maximum productivity from
the DSC autosampler is achieved when paired with our intelligent Advantage™ software, that permits
pre-programmed analysis, comparison, and presentation of results.
*U.S. Patent No. 6,644,136; 6,652,015; 6,760, 679; 6,823,278
Standard
Temperature (°C) -180 to 600 -180 to 725 -180 to 725 -180 to 725 -180 to 725
Pressure 100 kPa 100 kPa 100 kPa 100 kPa 100 kPa
Hermetic
Temperature (°C) -180 to 600 -180 to 600 -180 to 725 -100 to 250 Amb. to 250
Pressure 300 kPa 300 kPa 600 kPa 3.7 MPa 10 MPa
Q10P PRESSURE DSC MODULE
The Q10P is a dedicated pressure DSC system that provides heat flow
measurements on pressure sensitive materials from -130 to 725 ˚C,
at pressures from 1 Pa (0.01 torr) to 7 MPa (1,000 psi). The cell employs
standard heat flux DSC technology and incorporates pressure control
valves, a pressure gauge, and over-pressure protection. The pressure
DSC cell is also an accessory for the Q1000 DSC and can be used as a
standard cell from -180 to 725 ˚C.
PHOTOCALORIMETER
The Photocalorimeter Accessory (PCA), for the
Q1000 and Q100 DSC, permits characterization
of photocuring materials between -50 and 80 ˚C.
UV/Visible light (250-600 nm) from a high
pressure mercury source is transmitted to the
sample chamber via an extended range, dual-
liquid light guide with neutral density or band
pass filters. Tzero™ technology permits direct
measurement of light intensity. It also provides
for simultaneous measurement of two samples.
The PCA can also be equipped with a dual quartz
light guide for operation up to 250 ˚C.
Q SERIES™ ACCESSORIES 9
T E M P E R AT U R E C O N T R O L O P T I O N S
LIQUID NITROGEN
COOLING SYSTEM
The Liquid Nitrogen Cooling System (LNCS)
provides the highest performance and greatest
flexibility in cooling. It has the lowest operational
temperature (to -180 °C), greatest cooling rate capacity
(to 140 °C/min), and an upper temperature limit of
550 °C. It is ideal for isothermal crystallization
studies. The LNCS uses liquid nitrogen efficiently,
thus reducing operating costs. Its autofill capability
allows the LNCS to be automatically refilled from a
larger liquid nitrogen source for continuous DSC
operation. The LNCS is available for the Q1000,
Q100, and Q10 DSC modules.
FINNED AIR COOLING SYSTEM
The Finned Air Cooling System (FACS) is an innovative cooling accessory for the Q1000, Q100, and Q10
DSC modules that offers a cost-effective alternative to the refrigerated and liquid nitrogen cooling systems.
The FACS can be used for controlled cooling experiments, thermal cycling studies, and to improve sample
turnaround time. It uses compressed air to cool the DSC cell. Stable baselines and linear heating and
cooling rates can be achieved between ambient and 725 °C. A special version of the Quench Cooling
Accessory is available for use with the FACS to speed cooling of the DSC cell to ambient temperatures.
T E M P E R AT U R E C O N T R O L O P T I O N S 11
TZER O™ DSC TECHNOLOGY
• Essentially flat baselines with better than an order of magnitude improvement on other designs,
especially in the subambient temperature range
• Superior sensitivity due to flatter baselines and better signal-to-noise ratio
• Best available resolution (even over power compensation devices)
• Faster MDSC® experiments
• Direct measurement of heat capacity (Q1000)
Tzero* technology produces the truest available representation of heat flowing to and from a sample, by
removing instrumental thermal effects that degrade baseline flatness, sensitivity, and resolution in other
designs. The Tzero cell’s unique internal reference temperature sensor and electronic circuitry measure the
resistive and capacitive imbalances that cause these effects. An advanced four-term, heat flow expression
accounts for them, and also for known heating rate differences at the sample and reference that occur during
major thermal events (e.g., melting). Tzero technology is available on the Q1000 and the Q100. Advanced
Tzero (available only on the Q1000) compensates for pan contact resistance, thereby further improving
resolution and allowing direct heat capacity (Cp) measurements.
*U.S. Patent No. 6,431,747; 6,488,406; 6,523,998
∆T 1 1 dT d∆T
q=–
Rr
+ ∆T0 –
Rs Rr ( )
+ (Cr – Cs) s – Cr
dτ dτ
SENSITIVITY FIGURE 2
-0.2 10 ˚C/min
of polypropylene, whose Tg is not easily measured -17 ˚C
by DSC, even with a larger sample, due to its
highly crystalline nature. The data shows that the -0.3
Tg is easily detected even at a slow 5 °C/min
heating rate. The excellent Q1000 baseline is the -13 ˚C
20˚ C/min
-0.4
essential key for accurate measurements of glass
transitions and heat capacity from materials that -40 -30 -20 -10 0 10 20
exhibit weak and broad transitions. Temperature (˚C)
FIGURE 3
RESOLUTION 0
Q1000
Figure 3 shows a comparative resolution plot of Q100
indium performed on the Q Series DSC’s (Q1000, -5 Q10
T Z E R O ™ DSC P E R F O R M A N C E 13
M O D U L AT E D D S C ® T E C H N O L O G Y
In MDSC*, a sinusoidal temperature oscillation is overlaid on the traditional linear ramp. The net effect is that
heat flow can be measured simultaneously with changes in heat capacity. Using Fourier transformation,
the heat flow generated is separated in real time into a heat capacity component and a kinetic component.
In MDSC, the DSC heat flow is called the Total Heat Flow, the heat capacity component is the Reversing Heat
Flow, and the kinetic component is the Nonreversing Heat Flow. The Total Heat Flow signal contains the sum
of all thermal transitions, just as in standard DSC. The Reversing signal contains glass transition and melting
transitions, while the Nonreversing Heat Flow contains kinetic events like curing, volatilization, melting, and
decomposition. The Q1000 uniquely permits increased MDSC productivity of high quality data by its ability to
operate at standard DSC heating rates (e.g., 10 ˚C / min.).
*U.S. Patent Nos. 5,224,775; 5,248,199; 5,346,306
Canadian Patent No. 2,089,225 Japanese Patent No. 2,966,691
dH = Cp dT + f (t, T)
dt dt
Heat = Heat Capacity + Kinetic
Flow Component Component
SEPARATION OF FIGURE 4
sample. While the former is not easy to interpret, -43.66 ˚C Total Heat Flow -0.2
the reversing signal clearly indicates a Tg for sucrose -0.4 Reversing Heat Flow -41.54 ˚C(H)
-0.2
between -43.6 and -39.4 °C. The exothermic non-reversing -39.4 ˚C
-0.4
signal (peak max -36 °C; heat of crystallization 5.7 J/g)
Note; All curves at same Sensitivity
relates to crystallization of free water that could not -0.6 Sample quenched in liquid nitrogen -0.4
crystallize during quench cooling of the sample due to -0.6
a significant increase in mobility and diffusion of the -60 -50 -40 -30 -20
Temperature (˚C)
material at the glass transition.
MDSC ® A P P L I C AT I O N S 15
D S C A P P L I C AT I O N S
TRANSITION TEMPERATURES
DSC provides rapid and precise determinations of FIGURE 7
transition temperatures using minimum amounts of a
sample. Common temperature measurements include
HEAT FLOW
FIGURE 8
The DSC heat flow signal is commonly used to measure 6 275 ˚C 600
the following: 531 J/g
Heat Capacity (J/g/˚C)
Integral (J/g)
• Hazard Potential • Cure Rates Single Run 135 ˚C
0.731 J/g
• Lifetime Estimation • Kinetics 2
Running Integral
Figure 8 shows a single analysis measurement of total 200
0
heat and heat capacity (Cp) by advanced DSC
technology (see page 12). The heat capacity increases
-2 0
as the sample passes through its glass transition, cold 0 50 100 150 200 250 300
crystallization, and melting events. Temperature (˚C)
ENTHALPY 0.4
FIGURE 9
exo
methods include reaction induction time (E2046),
Size: 21 mg
oxidation induction time (OIT; D3895), and constant Atm: Oxygen
temperature stability (E487). Comparative OIT tests
Heat Flow
Prog: 200 ˚C ISO
permit relative ranking of the effectiveness of
different anti-oxidant packages in a given polymer.
As seen in Figure 10, the analyses are rapid, and
with relative performance quickly established,
endo
36 min
the antioxidant selection can be made on needs,
0 5 10 15 20 25 30 35 40
processing conditions, and relative cost. Time (min)
PHOTOCURING
FIGURE 12
The Photocalorimeter Accessory (PCA) provides a
convenient tool to assess reactions initiated with
UV/Visible light. Figure 12 compares two different
A
acrylic formulations under the same conditions. The
Heat Flow (mW)
DSC A P P L I C AT I O N S 17
NOTES
W W W. T A I N S T R U M E N T S . C O M
T–2006