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ECHNOLOGY, PERFORMANCE, VERSATILITY, AND RELIABILITY ARE WORDS THAT DESCRIBE A TA INSTRUMENTS Q SERIES™ DIFFERENTIAL SCANNING CALORIMETER (DSC). THE Q1000, Q100, Q10, AND Q10P ARE FIFTH-GENERATION PRODUCTS FROM THE WORLD LEADER IN DIFFERENTIAL SCANNING CALORIMETRY

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ECHNOLOGY, PERFORMANCE, VERSATILITY, AND RELIABILITY ARE WORDS THAT DESCRIBE A TA INSTRUMENTS Q SERIES™ DIFFERENTIAL SCANNING CALORIMETER (DSC). THE Q1000, Q100, Q10, AND Q10P ARE FIFTH-GENERATION PRODUCTS FROM THE WORLD LEADER IN DIFFERENTIAL SCANNING CALORIMETRY

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rajdeeps
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© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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TA Instruments

Q SERIES™ THERMAL ANALYZERS


TA I NSTRUMENTS , W ORLDWIDE
More worldwide customers choose TA Instruments than any competitor
as their preferred thermal analysis or rheology supplier. We earn this
distinction by best meeting customer needs and expectations for high
technology products, quality manufacturing, timely deliveries, excellent
training, and superior after-sales support.

SALES AND SERVICE


We pride ourselves in the technical competence and professionalism of our sales force, whose only business is rheology and
thermal analysis. TA Instruments is recognized worldwide for its prompt, courteous, and knowledgeable service staff.
Their specialized knowledge and experience are major reasons why current customers increasingly endorse our company and
products to their worldwide colleagues.

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

ECHNOLOGY, PERFORMANCE, VERSATILITY, AND RELIABILITY ARE WORDS

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

SCANNING CALORIMETRY. EACH REPRESENTS AN UNPARALLELED INVESTMENT

BECAUSE IT DELIVERS CUTTING-EDGE TECHNOLOGY, IS DESIGNED WITH THE

CUSTOMER IN MIND, AND IS BACKED BY SUPERIOR SUPPORT THAT IS THE

HALLMARK OF OUR COMPANY.

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

D IFFERENTIAL S CANNING C ALORIMETERS 3


DIFFERENTIAL SCANNING CALORIMETERS

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

Q1000 Q100 Q10 Q10P


Tzero™ Technology Advanced Basic Not Available Not Available

MDSC® Included Optional Not Available Not Available

Direct Cp Measurement Yes Not Available Not Available Not Available

Touch Screen Included Included Not Available Not Available

User-Replaceable Cell Yes Not Available Not Available Yes

Pressure DSC Cell Optional Not Available Not Available Yes

Photocalorimeter Optional Optional Not Available Not Available

Digital Mass Flow Controller Included Included Included Not Available

50-Position Autosampler Included Optional Not Available Not Available

Auto Lid Included Included Not Available Not Available

Temperature Accuracy ± 0.1 ˚C ± 0.1 ˚C ± 0.1 ˚C ± 0.1 ˚C

Temperature Precision ± 0.01 ˚C ± 0.05 ˚C ± 0.05 ˚C ± 0.05 ˚C

Temperature Range (with cooling accessory) -180 to 725 ˚C -180 to 725 ˚C -180 to 725 ˚C -130 to 725 ˚C

Calorimetric Precision (metal standards) ± 0.05% ± 1% ± 1% ± 1%

Sensitivity 0.2 µW 0.2 µW 1.0 µW 1.0 µW

Baseline Curvature with Tzero (-50 to 300˚C) 10 µW 10 µW Not Available Not Available

Baseline Reproducibility with Tzero ±10 µW ±10 µW <0.04 mW Not Available

Relative Resolution 2.9 2.1 1.0 1.0

T ECHNICAL S PECIFICATIONS 5
Q1000/Q100 TECHNOLOGY

TZERO CELL DESIGN


The Tzero™ cell is designed for excellence in both
heating and cooling operation. Its many innovations
include a new sensor with raised sample and
reference platforms. The sensor is machined for
symmetry from a single piece of durable, thin wall,
high response constantan and brazed to the silver
heating block. Benefits: Provides faster signal
response, flat baselines, superior sensitivity and
resolution, plus improved data precision.
A new chromel/constantan Tzero thermocouple is
located midway between the sample and reference sensor platforms. Benefits: It provides for independently
measured sample and reference heat flows that produce superior DSC and MDSC® results. It simultaneously
acts as a control sensor to assure precise isothermal furnace operation.
Matched chromel area thermocouples are welded to the underside of each sensor platform and provide
superior performance to other thermocouple designs. Benefits: High sensitivity detection of any temperature
transition that results from a physical change in the sample.

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

COOLING RODS & RING


The innovative design features an array of 54 symmetrically arranged, high conductivity, nickel cooling rods
that connect the silver furnace with the cooling ring. Benefits: This provides superior cooling performance
over a wide temperature range. High cooling rates and instantaneous turnaround from heating to cooling are
now achievable. Lower subambient temperatures and unmatched baseline performance can now be obtained
with our range of cooling accessories in isothermal, programmed cooling, and MDSC® experiments.
Turnaround time between experiments is dramatically reduced.

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.

Platinel™ is a trademark of Englehard Industries

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

DSC SAMPLE PANS


TA Instruments offers a wide selection of
sample pans to meet multiple standard
and specialized applications. These include
aluminum, alodined aluminum, copper, gold,
platinum, graphite and stainless steel. They
can be used under a variety of temperature
and pressure conditions. Samples can be run
in the standard DSC mode in open pans,
crimped or hermetically sealed pans / lids or
in pressure capsules. Samples in open pans can also be run at controlled pressures using the PDSC Cell.
All aluminum standard pans have the same temperature and pressure rating. General details of the pans are
as follows:

Standard

Aluminum Copper Platinum Gold Graphite

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

Aluminum Alodined Aluminum Gold Hi Volume Pressure

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.

MASS FLOW CONTROLLERS


High quality DSC experiments require precise
purge gas flow rates, especially when using high
conductivity gases, such as helium. Mass flow
controllers, along with integrated gas switching,
provide flexible control as part of individual
methods. Purge gas flow rates are settable from
0-240 mL/min in increments of 1 mL/min.
The system is precalibrated for helium, nitrogen,
air and oxygen and suitable calibration factors
may be entered for other gases.

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

REFRIGERATED COOLING SYSTEM


The Refrigerated Cooling System (RCS) is
frequently selected as the cooling device of choice
for trouble-free, unattended DSC and MDSC™
operation. It operates from -90 °C to 550 °C using a
two-stage, closed, evaporative refrigerator system.
Because it is a sealed system requiring only
electrical power, the RCS is frequently preferred for
operation in areas where other refrigerants, such as
liquid nitrogen, are difficult or expensive to obtain.
The RCS is compatible with Q1000, Q100, and
Q10 DSC modules.

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.

QUENCH COOLING ACCESSORY


The Quench Cooling Accessory (QCA) is a manually operated cooling accessory that is a cost-effective
alternative to the automated RCS or LNCS. Its primary use is with the Q10 DSC to quench cool a sample to
a subambient temperature prior to heating to an upper limit. Since active cooling is not present in QCA
experiments, the T1 signal is the measured entity. The recommended temperature of operation of the QCA is
from –180 to 400 °C. The QCA reservoir is easily filled with ice water, liquid nitrogen, dry ice, or other
cooling mixtures.

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

TZERO™ TECHNOLOGY PROVIDES:

• 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

Principle Thermal Thermal Heating


Heat Resistance Capacitance Rate
Flow Imbalance Imbalance Imbalance
TZER O™ DSC PERFORM ANCE

BASELINE STABILITY (FLATNESS) 0.5


FIGURE 1

Figure 1 shows a comparison of a Q1000 empty Heat Flow Q1000


Heat Flow STD DSC
cell baseline with that from a high performance,
0.25
non-Tzero, heat flux DSC. The data shows that the

Heat Flow (mW)


Q1000 baseline is superior in every way. The start-
up offset is much smaller, the baseline is 0.00

dramatically straighter, and the slope is greatly


reduced. Notice the heat flow scale, and that the -0.25
signal is almost zero throughout the -80 to 400 °C
temperature range. This also contrasts markedly -0.5
with results from other DSC designs, where a -100 25 150 275 400
Temperature (˚C)
baseline bow of 1 mW over the same temperature
range is often considered acceptable.

SENSITIVITY FIGURE 2

Figure 2 shows a Q1000 high sensitivity glass -0.1 5 ˚C/min


transition (Tg) measurement, as a function of -18 ˚C
heating rate, for a very small (1 mg) sample
Heat Flow (mW)

-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

Q100, and Q10) under identical conditions. The


Heat Flow (mW)

Q10 data is typical of a good performing DSC -10

system without Tzero™ technology. The improve-


ments seen in the Q1000 and Q100 are impressive -15

displays of the power of Tzero™ technology in the


-20
steeper leading edge trace and in the subsequent
faster return to baseline. This is especially true in
-25
the Q1000, which outperforms power-compensated 155 156 157 158 159 160 161
DSC models in recognized resolution tests. Temperature (˚C)

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

MDSC® TECHNOLOGY PROVIDES:

• Separation of complex transitions into more easily


interpreted components

Modulated Temperature (˚C)


• Increased sensitivity for detecting weak transitions and melts
• Increased resolution without loss of sensitivity
• Direct measurement of heat capacity
• More accurate measurement of crystallinity Temperature (˚C)

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

Total Heat = Reversing + Nonreversing


Flow Heat Flow Heat Flow
M D S C ® A P P L I C AT I O N S

SEPARATION OF FIGURE 4

COMPLEX TRANSITIONS -0.10


Non Rev Heat Flow
Figure 4 shows MDSC® results for a copolymer of -0.11

Heat Flow (mW)


polyethylene terephthalate and acrilonitrile/butadiene/
styrene (PET/ABS) when analyzed over the temper- -0.12 Total Heat Flow
ature range from ambient to 170 ˚C. The MDSC total
-0.13
heat flow signal shows only the PET glass PET Tg
transition and cold crystallization, with no evidence of -0.14 ABS Tg Rev Heat Flow
the ABS. The reversing heat flow clearly identifies
glass transitions for both PET and ABS. The non- -0.15
20 40 60 80 100 120 140 160 180 200
reversing trace indicates the cold crystallization peak Temperature (˚C)
for PET, plus an enthalpic relaxation resulting from the
sample’s previous history.

IMPROVED SIGNAL SENSITIVITY FIGURE 5


Figure 5 shows the improved sensitivity of MDSC for
measuring very broad and weak transitions, such as
glass transitions in highly crystalline polymers or where Total Heat Flow
Heat Flow (mW)

the Tg is hidden beneath a second overlapping thermal


event. This data was generated using a very small
(2.2 mg) sample of a polymer coating. The total heat
Reversing Heat Flow 109 ˚C (H)
flow shows no transitions in the region where a Tg 0.009 mW
would be expected, though the large endotherm
around 40 °C indicates solvent loss. The Reversing
Heat Flow does indicate a very weak (8.5 µW) 0 20 40 60 80 100 120 140
Tg around 109 °C, illustrating the sensitivity of the Temperature (˚C)
MDSC technique.

IMPROVED DATA INTERPRETATION


Figure 6 shows an application of interest in studies FIGURE 6
of foods or pharmaceuticals, in which the MDSC total -36.08 ˚C Nonreversing 0.0
heat flow signal and its reversing and non-reversing Nonreversing Heat Flow Heat Flow (mW)
-0.2 5.704 J/g 0.0
components are displayed for a 40% aqueous sucrose
Rev. Heat Flo (mW)
Heat Flow (mW)

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 –> exothermic


the following: Oxidation
or
Decomposition
• Melting • Crystallization
Melting
• Glass Transition • Polymorphic Transition Glass
Transition Crystallization Cross-Linking
• Thermal Stability • Liquid Crystal (Cure)
• Oxidation Onset • Protein Denaturation
• Cure Onset • Solid-Solid Transition
Figure 7 shows typical shapes for the main transitions Temperature
observed in DSC.

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)

• Specific Heat Capacity • Glass Transition 4


Heat Capacity, 400

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

Heat flow signal integration gives quantitative enthalpy


information about the transition. For example: 0.2 Enthalpy 114.8 J/g
Heat Flow (mW/mg)

• Heat of Fusion • Explosion Potential 0.0


• Percent Crystallinity • Degree of Cure
• Heat of Crystallization • Heat of Reaction -0.2

Figure 9 The DSC plot of a thermosetting resin allows -0.4

determination of the heat of reaction and degree of


cure. Specialty kinetics software can also provide the -0.6
125 175 225 275
reaction order, activation energy, and reaction rates. Temperature (˚C)
TIME
FIGURE 10
Kinetics is the study of the effects of time and
temperature on a reaction. Common ASTM test

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)

PRESSURE (AND TIME) FIGURE 11


Pressure DSC accelerates OIT analyses and 0.6
“sharpens” the onset of the oxidation process. Sample A
Sample B
Figure 11 shows a comparative study of a series of 0.4
Sample C
Sample D
two component polymer dispersions containing
Heat Flow (W/g)

different levels of the same antioxidant. Clear


0.2
performance differences are readily seen. The tests
provided the same answer in under two days that
0.0
took up to two months of traditional “field exposure”
to obtain. Other common PDSC applications include
a) thermoset resin cures, b) catalyst studies, and -0.2
0 50 100 150 200 250
c) micro-scale simulations of chemical reactions. 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)

data shows that formulation A cures rapidly upon


exposure to UV radiation, while formulation B reacts
slower, and has both a longer time-to-peak and
B
lower energy. In all PCA experiments, the peak
shapes and transition energies are affected by the
formulation chemistry, additives, initiators, and the 0 1 2 3 4 5
purge gas used. Time (min)

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

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