dsc2010 user manual

iTA INSTRUMENTS DSC 2010

DSC 2010

Differential Scanning Calorimeter

Operator’s Manual

PN 925604.001 Rev. E (Text and Binder)PN 925604.002 Rev. E (Text Only)Issued May 1998

TA Instruments 109 Lukens Drive New Castle, DE 19720

Thermal Analysis & Rheology

A SUBSIDIARY OF WATERS CORPORATION

ii TA INSTRUMENTS DSC 2010

©1995, 1996, 1997, 1998 by TA Instruments109 Lukens DriveNew Castle, DE 19720

Notice

The material contained in this manual is be-lieved adequate for the intended use of thisinstrument. If the instrument or procedures areused for purposes other than those specifiedherein, confirmation of their suitability must beobtained from TA Instruments. Otherwise, TAInstruments does not guarantee any results andassumes no obligation or liability. This publica-tion is not a license to operate under or arecommendation to infringe upon any processpatents.

TA Instruments Operating Software and Instru-ment, Data Analysis, and Utility Software andtheir associated manuals are proprietary andcopyrighted by TA Instruments, Inc. Purchasersare granted a license to use these softwareprograms on the instrument and controller withwhich they were purchased. These programsmay not be duplicated by the purchaser withoutthe prior written consent of TA Instruments.Each licensed program shall remain the exclu-sive property of TA Instruments, and no rightsor licenses are granted to the purchaser otherthan as specified above.

iiiTA INSTRUMENTS DSC 2010

Table of ContentsNotes, Cautions, and Warnings.................ix

Safety.............................................................x

Using This Manual......................................xv

CHAPTER 1: Introducingthe DSC 2010............................................. 1-1

Introduction................................................. 1-3

Components ............................................. 1-5

The 2010 Instrument ................................... 1-6

2010 Instrument Keypad ......................... 1-7POWER Switch ................................ 1-9

2010 DSC Cell ......................................... 1-9

Accessories ............................................... 1-10

Sample Encapsulating Press ............... 1-10Accessories forSubambient Operation ........................ 1-11

LNCA.............................................. 1-11RCS ................................................. 1-12DSC Cooling Can ........................... 1-13

Specifications ............................................ 1-14

iv TA INSTRUMENTS DSC 2010

Table of Contents(continued)

CHAPTER 2: Installing theDSC 2010................................................... 2-1

Unpacking/Repacking the 2010 ................. 2-3

Unpacking the 2010 ................................ 2-3

Unpacking the DSC Cell ......................... 2-6

Repacking the 2010 ................................. 2-6

Installing the 2010 Instrument .................... 2-7

Inspecting the System.............................. 2-7

Choosing a Location ............................... 2-8

Connecting Cables and Gas Lines .......... 2-9

GPIB Cable .......................................... 2-9Purge, Vacuum,and Cooling Gas Lines ....................... 2-12

PURGE Line ................................... 2-12VACUUM Line .............................. 2-13COOLING GAS Line ..................... 2-13

Power Cable ....................................... 2-15

Installations for Subambient Operation ... 2-16

Installing the DSC Cooling Can............ 2-17

Starting the 2010....................................... 2-20

Shutting Down the 2010 ........................... 2-21

vTA INSTRUMENTS DSC 2010


CHAPTER 3: Running Experiments...... 3-1

Overview ..................................................... 3-3

Before You Begin .................................... 3-3

Calibrating the DSC.................................... 3-4Baseline Slope and Offset Calibration .... 3-5Cell Constant Calibration ........................ 3-6Temperature Calibration ......................... 3-6

Running a DSC Experiment ....................... 3-7

Experimental Procedure .......................... 3-7

Preparing Samples ................................... 3-8Determining Sample Size ..................... 3-8Physical Characteristics ....................... 3-9Selecting Sample Pans ......................... 3-9

Sample Pan Material ......................... 3-9Sample Pan Configuration .............. 3-11

Nonhermetic Pans ........................ 3-11Hermetic Pans .............................. 3-11Open Pans .................................... 3-12SFI Pans ....................................... 3-12

Encapsulating the Sample .................. 3-12Preparing NonhermeticSample Pans .................................... 3-13Preparing HermeticSample Pans .................................... 3-16

Setting Up Accessories ...................... 3-19

Loading the Sample ............................ 3-21

vi TA INSTRUMENTS DSC 2010


Starting an Experiment .......................... 3-23

Stopping an Experiment ........................ 3-23

Subambient Experiments .......................... 3-24

DSC Cooling Can .................................. 3-24Applications ....................................... 3-24Operation ............................................ 3-25

Quench-CoolingBetween Runs ................................. 3-25

Starting a Run BelowAmbient Temperature ..................... 3-26

Programmed Cooling ...................... 3-26

CHAPTER 4: Technical Reference......... 4-1

Description of the DSC 2010...................... 4-3

DSC Cell .................................................. 4-3

Principles of Operation ............................... 4-5

Cell Block Heating .................................. 4-5

Sample and Reference Thermocouples ... 4-6

DSC Applications ....................................... 4-7

Sample Types .......................................... 4-7

Status Codes ............................................... 4-8

viiTA INSTRUMENTS DSC 2010


Guidelines for Quantitative Studies .......... 4-12

Specific Heat Experiments .................... 4-12

CHAPTER 5: Maintenanceand Diagnostics......................................... 5-1

Overview ..................................................... 5-3

Routine Maintenance .................................. 5-4

Inspection ................................................ 5-4

Cleaning the Instrument Keypad ............. 5-4

Cleaning a Contaminated Cell ................. 5-4

Cleaning DSC Pans ................................. 5-5

Sample Encapsulating Press .................... 5-7

Diagnosing Power Problems ....................... 5-8

Fuses ........................................................ 5-8

Power Failures ......................................... 5-9

DSC 2010 Test Functions ......................... 5-12

2010 Confidence Test ............................ 5-12

Replacement Parts .................................... 5-13

viii TA INSTRUMENTS DSC 2010


Appendix A: SampleEncapsulating Press.................................A-1

Appendix B: OrderingInformation ..............................................B-1

Index ...........................................................I-1

ixTA INSTRUMENTS DSC 2010

Notes, Cautions,and Warnings

This manual uses NOTES, CAUTIONS, andWARNINGS to emphasize important andcritical instructions.

A NOTE highlights important information aboutequipment or procedures.

A CAUTION emphasizes a procedure that maydamage equipment or cause loss of data if notfollowed correctly.

A WARNING indicates a procedure thatmay be hazardous to the operator or to theenvironment if not followed correctly.

NOTE:

ttttt CAUTION:

!WARNING

x TA INSTRUMENTS DSC 2010

SafetyThis equipment has been designed to complywith the following standards on safety:

• IEC 1010-1/1990 and A1/1992• IEC 1010-2-010/1992• EN 61010-1/1992• EN 61010-2-010/1994• UL 3101-1, First Edition.

Electrical Safety

You must unplug the instrument before doingany maintenance or repair work; voltagesexceeding 110 volts AC are present in thissystem.

High voltages are present in this instru-ment. If you are not trained in electricalprocedures, do not remove the cabinetcovers. Maintenance and repair of internalparts must be performed only by TA Instru-ments or other qualified service personnel.

After transport or storage in humid condi-tions, this equipment could fail to meet allthe safety requirements of the safetystandards indicated. Refer to the NOTE onpage 2-8 for the method used to dry outthe equipment before use.

!WARNING

!WARNING

xiTA INSTRUMENTS DSC 2010

Potential Asphyxiant

Liquid nitrogen can cause rapid suffocation withoutwarning.

Store and use in an area with adequate ventilation.

Do not vent LNCA container in confined spaces.

Do not enter confined spaces where nitrogen gasmay be present unless the area is well ventilated.

The warning above applies to the use of liquid nitrogen. Oxygendepletion sensors are sometimes utilized where liquid nitrogen isin use. Please refer to the “Safety” section of the TA Instru-ments Liquid Nitrogen Cooling Accessory manual for more de-tailed instructions regarding the use of the LNCA.

WARNING

xii TA INSTRUMENTS DSC 2010

Safety(continued)

Handling Liquid Nitrogen

The DSC 2010 uses the cryogenic (low-tempera-ture) agent, liquid nitrogen, for cooling. Be-cause of its low temperature (-195°C), liquidnitrogen will burn the skin. When you workwith liquid nitrogen, use the following precau-tions:

Liquid nitrogen evaporates rapidly at roomtemperature. Be certain that areas whereliquid nitrogen is used are well ventilated toprevent displacement of oxygen in the air.

1. Wear goggles or a face shield, gloves largeenough to be removed easily, and a rubberapron. For extra protection, wear high-topped, sturdy shoes, and leave your pantlegs outside the tops.

2. Transfer the liquid slowly to prevent thermalshock. Use containers that have satisfactorylow-temperature properties. Ensure thatclosed containers have vents to relievepressure.

3. The purity of liquid nitrogen decreases asthe nitrogen evaporates. If much of theliquid in a container has evaporated, analyzethe remaining liquid before using it for anypurpose where high oxygen content could bedangerous.

!WARNING

xiiiTA INSTRUMENTS DSC 2010

!WARNING

ttttt CAUTION:

!WARNING

Safety(continued)

IF A PERSON IS BURNED BY LIQUIDNITROGEN . . .

1. IMMEDIATELY flood the area (skin oreyes) with large quantities of cool water,and then apply cold compresses.

2. If the skin is blistered or if there is achance of eye infection, take the personto a doctor IMMEDIATELY.

Chemical Safety

Do not use hydrogen or any other explosivegas with the DSC 2010.

Use of chlorine gas will damage the cell.

Some samples may give off hazardousgases when heated. Make sure that theDSC 2010 is well ventilated. Use a labo-ratory hood or exhaust hose to ventilategases.

Thermal Safety

After running an experiment, you must allow theDSC Cell to cool down before you touch theinternal cell surfaces. These surfaces can be hotenough to burn the skin during a sample run.

xiv TA INSTRUMENTS DSC 2010

!

Safety(continued)

Lifting the Instrument

The DSC 2010 is a fairly heavy instrument. Inorder to avoid injury, particularly to the back,please follow this advice:

Use two people to lift and/or carry theinstrument. The instrument is too heavyfor one person to handle safely.

!WARNING

xvTA INSTRUMENTS DSC 2010

Using This ManualChapter 1 Describes the 2010

instrument and itsspecifications.

Chapter 2 Describes how to connectthe 2010 instrument to therest of your system.

Chapter 3 Describes how to runDSC experiments.

Chapter 4 Provides technicalinformation and explainsthe DSC principles ofoperation.

Chapter 5 Describes instrumentmaintenance proceduresand lists replacementparts.

Appendix A Explains how to changethe Sample EncapsulatingPress dies.

Appendix B Lists worldwide TAInstrumentsoffices that you cancontact to placeorders, receive technicalassistance, and requestservice.

Index Lists the page numbers ofimportant topics for yourreference.

xvi TA INSTRUMENTS DSC 2010

TA INSTRUMENTS DSC 2010 1–1

CHAPTER 1: Introducing theDSC 2010

Introduction................................................. 1-3

Components ............................................. 1-5

The 2010 Instrument ................................... 1-6

2010 Instrument Keypad ......................... 1-7POWER Switch ................................ 1-9

2010 DSC Cell ......................................... 1-9

Accessories ............................................... 1-10

Sample Encapsulating Press ............... 1-10Accessories forSubambient Operation ........................ 1-11

LNCA.............................................. 1-11RCS ................................................. 1-12DSC Cooling Can ........................... 1-13

Specifications ............................................ 1-14

Introducing the DSC 2010

1–2 TA INSTRUMENTS DSC 2010


Introduction

IntroductionThe Differential Scanning Calorimeter (DSC)2010 (Figure 1.1) determines the temperatureand heat flow associated with material transi-tions as a function of time and temperature. Italso provides quantitative and qualitative dataon endothermic (heat absorption) and exother-mic (heat evolution) processes of materialsduring physical transitions that are caused byphase changes, melting, oxidation, and otherheat-related changes. This information helpsthe scientist or engineer identify processing andend-use performance.

The DSC 2010 instrument works in conjunctionwith a controller and associated software tomake up a thermal analysis system.

Your controller is a computer that performs thefollowing functions:

• Provides an interface between you and theanalysis instrument

• Enables you to set up experiments and enterconstants

• Stores experimental data• Runs data analysis programs.



Figure 1.1DSC 2010 withTA InstrumentsThermal Analyzer


Components

The DSC 2010 (see Figure 1.2) has two majorparts: the 2010 instrument, which contains thesystem electronics, and the cell, which containsits own thermocouples (temperature sensors) formonitoring differential heat flow and tempera-tures. The 2010 DSC cell is not interchangeablewith other cells or cell types. However, ifnecessary, the cell can be replaced by qualifiedservice personnel.

Figure 1.2DSC 2010

Introduction



The 2010 InstrumentThe 2010 instrument contains the electronicsand software needed to perform experiments andstore experimental results. The battery backed-up RAM in the instrument saves parametersvital to system operations if power is inter-rupted. Also contained in the instrument is aGPIB interface for communication with thecontroller.

The keypad on the front of the 2010 instrumentenables you to start and stop experiments.

The 2010 instrument also contains several hook-ups for other components and accessories in thethermal analysis system, including:

• Gas purge line• Cooling gas line• Vacuum line• LNCA (Liquid Nitrogen Cooling

Accessory)• Gas Switching Accessory• EVENT switch• GPIB (General Purpose Interface Bus)• Power cable.


2010 Instrument Keypad

The instrument keypad (see Figure 1.3) containskeys that control local operations at the instru-ment.

Experiment information and instrument constantsare entered from the controller keyboard, not theinstrument keypad.

Table 1.1 explains the functions of the instru-ment keys.

Figure 1.32010 DSCInstrument Keypad

The 2010 Instrument

NOTE:

READY LIGHT POWER LIGHT

START KEYSTOP KEY



Table 1.12010 InstrumentKeypad Function Keys

Key/Function Explanation

START Initiates the experimentafter checking themethod and the cell.This is the same functionas Start on the controller.

STOP If an experiment isrunning, this key ends themethod normally, asthough it had run to com-pletion; i.e., the method-end conditions selectedgo into effect, and thedata that has been gener-ated is saved. This is thesamefunction as Stop onthe controller.

If an experiment is notrunning (the instrument isin a stand-by or method-end state), the STOP keyhalts any activity (air cool,LNCA auto-fill, etc.).


The 2010 Instrument

POWER SwitchThe POWER switch on the back of the instru-ment turns the power to 2010 instrument on andoff. The green power light on the front panelshows that the instrument is ON. The yellowlight shows when the instrument is ready.

2010 DSC Cell

The 2010 DSC cell (Figure 1.4) is used tomeasure differential heat flow. The sample anda reference are materials placed in pans that siton raised platforms on a constantan disc, andheat is transferred through the disc up into thesample and reference. The differential heat flowis monitored by thermocouples beneath the disc.

Figure 1.42010 DSC Cell



Accessories

Sample Encapsulating Press

The TA Instruments Sample EncapsulatingPress (Figure 1.5) is used to prepare encapsu-lated samples for DSC experiments. It comeswith two sets of dies, one for hermetic and onefor nonhermetic sealing.

Figure 1.5Sample Encapsulating Press


Accessories forSubambient Operation

The DSC 2010 can be operated at below-ambient temperatures using one of three acces-sories: the Liquid Nitrogen Cooling Accessory(LNCA), the Refrigerated Cooling System(RCS), or the DSC Cooling Can.

LNCAThe LNCA (Figure 1.6) achieves automatic andcontinuous programmed sample cooling withinthe range of -150°C to 725°C when used withthe DSC Heat Exchanger installed on the DSCCell (refer to Chapter 2 for installation). Heat-ers vaporize the liquid nitrogen in the LNCAtank, and then the vapor collects and passesthrough a U-shaped tube to the bottom of thetank, where it is cooled by the surroundingliquid. The cooled gas is forced up and mixedwith liquid nitrogen. The gas/liquid mix isdelivered to the Heat Exchanger to cool the cell.

You can easily gain access to your samples withthe LNCA by simply removing the lids on theDSC Heat Exchanger.

Figure 1.6LNCA

Accessories



Refrigerated CoolingSystem (RCS)

The Refrigerated Cooling System (RCS), whichis used to cool DSC experiments, consists of atwo-stage, cascade, vapor compression refrigera-tion system with an attached cooling head. Thecooling head fits over the RCS-DSC cell for usewith the DSC 2010. The RCS can be used forexperiments requiring cooling within an operat-ing range of -70°C to 400°C. The maximum rateof cooling depends on the temperature range ofyour experiment.

Figure 1.7Refrigerated CoolingSystem


DSC Cooling Can

The DSC Cooling Can fits over the standardDSC Cell and has a reservoir into which you canplace coolant to cool the cell. Either quenchcooling or manual programmed cooling can beperformed. The manual programmed coolingrequires operator maintenance of the coolantlevel in the reservoir.

Figure 1.8DSC Cooling Can

Accessories

Open-top Bell Jar

Aluminum Spacer

Cooling Can

Split O-ring

DSC Cell



SpecificationsTables 1.2 through 1.3 contain the technicalspecifications for the 2010 instrument.

Table 1.22010InstrumentSpecifications

Dimensions Depth 65.5 cm (25.8 in.)Width 28.5 cm (11.3in.)Height 40.0 cm (15.7 in.)

Weight 20 kg (44 lb)(approx.)

Power 115 volts AC +10%50/60 Hz

Table 1.32010 DSC CellSpecifications

Heating Room temperatureTemperature to 725oC (inertRange atmosphere above

600oC) as supplied.

Cooling -150oC to 725°CTemperature with the LNCA and Range DSC Cooling Can,

-70°C to 400°Cwith the RCS.

Cooling rate Dependent onaccessory used andtemperature range

Sample size 0.5 to 100 mg(nominal)

(table continued)


Specifications

Table 1.3(continued)

Sample volume 10 mm3 in hermeticpans

Sample pans Various open orhermetically sealed

Atmosphere Atmospheric to 266Pa (2 torr);preheated dynamicgas purge (in excessof 100 mL/min)

Purge Gases Recommended:air, argon, helium,nitrogen, or oxygen

Typical flow rate 25-50 mL/min

Cell volume 2 cm3

Temperature +0.1°C repeatability

Differential CHROMEL®*-thermocouples constantan

Sample thermocouple CHROMEL®*-ALUMEL®*

Control thermocouple Platinel II**

Calorimetric 1 µW (rms)sensitivity

(table continued)

* CHROMEL® and ALUMEL® are registeredtrademarks of the Hoskins Manufacturing Company.

**Platinel is a registered trademark of EngelhardIndustries.




Constant +2.5% from -100 tocalorimetric 500oCsensitivity

Calorimetric 1% (based onprecision metal samples)

Baseline noise 0.5 µW (rms)


CHAPTER 2: Installation

Unpacking/Repacking the 2010 ................. 2-3

Unpacking the 2010 ................................ 2-3

Unpacking the DSC Cell ......................... 2-6

Repacking the 2010 ................................. 2-6

Installing the 2010 Instrument .................... 2-7

Inspecting the System.............................. 2-7

Choosing a Location ............................... 2-8

Connecting Cables and Gas Lines .......... 2-9

GPIB Cable .......................................... 2-9Purge, Vacuum,and Cooling Gas Lines ....................... 2-12

PURGE Line ................................... 2-12VACUUM Line .............................. 2-13COOLING GAS Line ..................... 2-13

Power Cable ....................................... 2-15

Installations for Subambient Operation ... 2-16

Installing the DSC Cooling Can ............ 2-17

Starting the 2010....................................... 2-20

Shutting Down the 2010 ........................... 2-21


Installation


Unpacking/Repackingthe 2010

These instructions are also found as separateunpacking instructions in the shipping box.

Refer to Figures 1 to 3 while unpacking yourinstrument.

Unpacking the 2010

Have an assistant help you unpack thisunit. Do not attempt to do this alone.

Figure 2.1Shipping Boxes

1. Open the shipping carton and remove theaccessory box.

NOTE:

!WARNING

Unpacking/Repacking the 2010


Installation

2. Remove the cardboard packing insert.

3. Stand at one end of the box with yourassistant facing you at the other end. Liftyour end of the unit out of the box as yourassistant lifts his/her end.

4. Place the unit on a lab bench with one sidehanging over the edge of the bench (seeFigure 2.2). Someone must be holdingonto the unit at all times while it is in thisposition.

Figure 2.2Removing the Plywood Board


5. While your assistant holds the unit, use awrench to remove the two nuts and washersfrom the bottom. Then lift and rotate theunit so that the other end hangs over theedge of the bench. Someone must holdonto the unit at all times while it is in thisposition. While your assistant holds theunit, remove the two nuts and washers fromthe other side.

6. Slide the unit completely onto the lab bench.Have your assistant hold one side up whileyou unscrew and remove the black rubbershipping feet from the bottom. Then rotatethe unit and remove the shipping feet fromthe other side in the same manner.

7. Have your assistant lift one side of the unitwhile you install two mounting feet on oneside (see Figure 2.3). Screw in about 1/4-inch of the threaded mounting post into theunit. Rotate the unit and install the tworemaining mounting feet in the same man-ner.

8. Have your assistant lift the entire unit whileyou slide the plywood board out from underit.

Figure 2.3Installing theMounting Feet

Unpacking/Repacking the 2010


Installation

Unpacking theDSC Cell

To unpack the DSC Cell on the 2010 instrument,follow the instructions below.

1. Remove the hold-down screws from theDSC bell jar shipping clamp. Remove theclamp. Install plugs (supplied in the acces-sory kit) into the holes.

2. Remove the bell jar from the cell. Removeand discard all packing material, such astape and polyethylene film.

3. Place the silver lid and cell cover (found inthe accessory kit) over the cell. The knobon the silver lid should be pointing up.Replace the bell jar over the cell.

Repackingthe 2010

To pack and ship your instrument, use thehardware retained during unpacking and reversethe instructions found on pages 2-3 to 2-6.


Installingthe Instrument

Before shipment, the 2010 instrument is inspect-ed both electrically and mechanically so that it isready for operation after it has been installed.Installation involves the following procedures,described in this chapter:

• Unpacking the 2010 instrument and itscomponents and accessory kit

• Inspecting the system for shipping damageand missing parts

• Connecting the instrument to the TAInstruments controller

• Connecting the gas and vacuum lines,accessories, and power cable.

If you wish to have your 2010 instrumentinstalled by a TA Instruments Service Represen-tative, call for an installation appointment whenyou receive your instrument.

Inspectingthe System

When you receive your 2010 instrument, lookover the instrument and shipping containercarefully for signs of shipping damage, andcheck the parts received against the enclosedshipping list.

If the instrument is damaged, notify the carrierand TA Instruments immediately.

If the instrument is intact but parts are missing,contact TA Instruments.

A list of TA Instruments offices can be found inAppendix B of this manual.

Installing the Instrument

Installing the DSC 2010


Choosinga Location

Because of the sensitivity of DSC experiments,it is important to choose a proper location forthe instrument. The 2010 instrument should be:

In . . . a temperature-controlled area.. . . a clean environment.. . . an area with ample working and ventilation

space. (Refer to the specifications inChapter 1 for the instrument’s dimensions.)

On . . . a stable work surface.

Near . . . a power outlet (115 volts AC, 50 or 60 Hz,15 amps). A step up/down line transformermay be required if the unit is operated at ahigher or lower line voltage.

. . . your TA Instruments controller.

. . . a compressed lab air and purge gas supplyfor use during cooling and subambientexperiments.

Away from . . . dusty environments.. . . exposure to direct sunlight.. . . direct air drafts (fans, room air ducts).. . . poorly ventilated areas.

Drying out the instrument may be needed if it hasbeen exposed to humid conditions. Certainceramic materials used in this equipment mayabsorb moisture, causing leakage currents toexceed those specified in the applicable standardsuntil moisture is eliminated. It is important thatthe instrument ground is adequately connected tothe facilities ground for safe operation.

Run this method to dry out the instrument:

1 Ramp at 10°C/min to 400°C2 Isothermal for 30 min.

NOTE:


Connecting Cablesand Gas Lines

To connect the cables and gas lines, you willneed access to the 2010 instrument’s rear panel.All directional descriptions are written on theassumption that you are facing the back of theinstrument.

Connect all cables before connecting thepower cords to outlets. Tighten thumbscrews onall computer cables.

Whenever plugging or unplugging power cords,handle them by the plugs, not by the cords.

Protect power and communications cable paths.Do not create tripping hazards by laying cablesacross accessways.

GPIB Cable

1. Locate the GPIB connector on the right rearof the 2010 instrument (see Figure 2.4).

2. Connect the GPIB cable to the connector.The GPIB cable is the only cable that fitsinto the connector.

3. Tighten the hold-down screws on theconnector.

4. Connect the other end of the GPIB cable tothe controller or to the GPIB cable ofanother instrument connected to the control-ler.




5. Select a unique address from 1 to 9 (one thatis not used by any other instruments orInstrument Interfaces connected to yourcontroller). Then use the binary addressswitches on the 2010 instrument connectorpanel to set the desired address (see Table2.1). Figure 2.5 shows a instrument addressof 7.

If you change the address after the instru-ment is powered on, you must press the resetbutton on the instrument to enter the newaddress.

Figure 2.42010 InstrumentConnector Panel

FUSE

FUSE



ADDRESS1 2 3 4 5O

N

Table 2.1Binary Address Settings*

Address Switch Pattern1 2 3 4 5

1 0 0 0 0 12 0 0 0 1 03 0 0 0 1 14 0 0 1 0 05 0 0 1 0 16 0 0 1 1 07 0 0 1 1 18 0 1 0 0 09 0 1 0 0 1

*0 = OFF; 1 = ON

Figure 2.5Binary Address Switches(Shown as Binary Address #7)



Purge, Vacuum, andCooling Gas Lines

PURGE Line

The PURGE gas is typically used to control theenvironment around the sample.

1. Locate the PURGE fitting on the right sideof the 2010 instrument back (see Figure2.6).

Figure 2.6PURGE andVACUUM Fittings

2. Make sure your purge source is regulatedbetween 5 and 30 psi and connected to aflow meter to regulate flow up to 150 mL/min.

Use of any explosive gas as a purge gas isdangerous and is not recommended for theDSC 2010 instrument.

Use of corrosive gases will shorten the life of theinstrument and the cell.

3. Connect the DSC 2010 purge fitting to asource of gas using a ¼-inch I.D. flexibletubing.

PurgeVacuum

!!!!!!WARNING

ttttt CAUTION:


VACUUM Line

The vacuum line will be needed if you are goingto perform subambient experiments. Connectthe line as follows:

1. Locate the VACUUM fitting on the rightside of the 2010 instrument back (see Figure2.6).

2. Connect the DSC 2010 VACUUM fitting toa source of dry nitrogen using 6.4 mm (¼-inch) I.D. flexible tubing.

To minimize moisture build-up during subambientexperiments, supply a dry nitrogen purge to thevacuum line using a rate of 100-150 ml/min.

COOLING GAS Line

If you intend to use cooling gas at the end of theexperiment, install a split O-ring to preventvibration of the bell jar. A split O-ring isprovided with the DSC Cooling Can. If you donot have a split O-ring, you can order one fromTA Instruments (see Appendix B) or cut the onethat comes with the DSC Cell.

O-rings are not used if the DSC 2010 is used withan automated cooling system such as the RCS orLNCA.

To connect the COOLING GAS line:

1. Locate the COOLING GAS fitting, a 6.4mm (¼-inch) compression fitting on the leftside of the 2010 instrument back, markedwith a 120 psi maximum warning label (seeFigure 2.7).

NOTE:

NOTE:




2. Make sure your cooling gas source isregulated between 20 and 120 psi.

The COOLING GAS line ties into a pressure-regulated valve that is set to 15 psi. The sourcepressure setting should not go below this value.

3. Connect a compressed air line to the COOL-ING GAS fitting.

Figure 2.7COOLING GAS Fitting

FUSE

FUSE

NOTE:

COOLING GAS FITTING

10 A


FUSE

FUSE

Power Cable

Connect all other cables and gas lines beforeconnecting the power cable to a wall outlet.

1. Make sure the 2010 instrument POWERswitch (see Figure 2.8) is in the OFF (0)position.

Figure 2.82010 InstrumentPOWER Switch

2. Plug the power cable into the 2010 instru-ment.

Before plugging the 2010 instrument powercable into the wall outlet, make sure the instru-ment is compatible with the line voltage. Checkthe label on the back of the unit to verify thevoltage.

3. Plug the power cable into the wall outlet.

NOTE:

POWER SWITCH


ttttt CAUTION:

10 A

Installation


Installations forSubambient Operation

The standard DSC Cell can be operated atsubambient conditions using any one of thefollowing cooling accessories:

• Liquid Nitrogen Cooling Accessory(LNCA) with the DSC Heat Exchanger

• Refrigerated Cooling System (RCS)• DSC Cooling Can.

This section describes how to install the DSCCooling Can accessory. The installation of theLNCA and the RCS with the DSC 2010 can befound in the literature accompanying thoseaccessories.


Installing the DSC Cooling Can

The DSC Cooling Can is a metal can that fitsover the DSC Cell. Coolant is placed in areservoir in the top of the can. An open-top belljar, a Teflon* disc, an aluminum spacer, and asplit O-ring are included with the accessory.

Figure 2.9Installing the Teflon Discin the DSC Cooling Can

The installations for quench and programmedcooling are the same, with one exception: theTeflon disc is used for programmed coolingonly. The disc is permanent once inserted, sothe DSC Cooling Can can be used for only onetype of cooling once it is installed: quench orprogrammed. Be sure to determine which typeof cooling you plan to use before you install thisaccessory.

The components installed in the following stepsare in the parts bag shipped with the DSCCooling Can:

1. Remove the bell jar from the DSC Cell.Remove the original O-ring and replace itwith the split O-ring shipped with the DSCCooling Can.

* Teflon is a registered trademark of the DuPont Com-pany.

Installations for Subambient Operation


Installation

2. If you plan to do programmed coolingexperiments with the DSC Cooling Can,first punch a 2-cm hole in the center of theinsulation disc. This allows you to removethe disc from the can later by prying up theedge of the hole with a tool. Place theinsulation disc inside the can by turning thecooling can upside down, putting the discinto the can, and pushing the disc until itsnaps into place (see Figure 2.9).

Once the Teflon disc is installed, you cannotremove it; the DSC Cooling Can will be set uppermanently for programmed cooling.

The insulation disc will soften at 325°C.

If you plan to do quench cooling experimentswith the DSC Cooling Can, do not install theTeflon disc.

NOTE:

ttttt CAUTION:


Figure 2.10Installing the DSCCooling Can

3. Place the aluminum spacer on top of the cellas shown in Figure 2.10.

4. Place the DSC Cooling Can over the DSCCell.

5. Place the open-top bell jar over the DSCCoolingCan.

When running subambient experiments, use a drynitrogen purge through the vacuum port (~100 –150 ml/min) and a dry gas through the purgeport to eliminate moisture buildup.

Installations for Subambient Operation

Open-top Bell Jar

DSC Cell

Aluminum Spacer

Cooling Can

Split O-ring

NOTE:


Installation

Starting the DSC 2010Allow the 2010 instrument to warm up for at least30 minutes before performing an experiment.

1. Check all connections between the 2010instrument and the controller. Make sureeach component is plugged into the correctconnector.

2. Press the instrument POWER switch,located on the rear of the instrument, to theON position. The green power light on thefront of the instrument should turn on andthe yellow Ready light should flash.

3. Make sure the green power light comes on;if it does not, recheck the power connectionsto the instrument and the power source. Ifthe connections are good, check the instru-ment power fuse F1 on the rear of theinstrument to see if the fuse is blown. If thefuse is blown, replace it, see Chapter 5.

You are now ready to start up the rest of thethermal analysis system.

NOTE:


Shutting Down the2010 Instrument

Before you decide to power down your 2010instrument, consider the following:

• All of the components of your thermalanalysis system are designed to be lefton for long periods.

• The electronics of the 2010 instrumentand the controller perform more reliablyif power fluctuations caused by turningunits on and off are minimized.

For these reasons, turning the system and itscomponents on and off frequently is dis-couraged.

When you finish running an experiment on your2010 instrument and wish to use the thermalanalysis system for some other task, leave theinstrument on; it will not interfere with whateverelse you wish to do.

If you do need to power down your 2010instrument for any reason, simply press thePOWER switch to the OFF position.

Shutting Down the 2010 Instrument


Installation


CHAPTER 3: Running Experiments

Overview ..................................................... 3-3

Before You Begin .................................... 3-3

Calibrating the DSC .................................... 3-4Baseline Slope and Offset Calibration .... 3-5Cell Constant Calibration ........................ 3-6Temperature Calibration ......................... 3-6

Running a DSC Experiment ....................... 3-7

Experimental Procedure .......................... 3-7

Preparing Samples ................................... 3-8Determining Sample Size ..................... 3-8Physical Characteristics ....................... 3-9Selecting Sample Pans ......................... 3-9

Sample Pan Material ......................... 3-9Sample Pan Configuration .............. 3-11

Nonhermetic Pans ........................ 3-11Hermetic Pans .............................. 3-11Open Pans .................................... 3-12SFI Pans ....................................... 3-12

Encapsulating the Sample .................. 3-12Preparing NonhermeticSample Pans .................................... 3-13Preparing HermeticSample Pans .................................... 3-16

Setting Up Accessories ...................... 3-19

Loading the Sample ............................ 3-21

Running Experiments


Starting an Experiment .......................... 3-23

Stopping an Experiment ........................ 3-23

Subambient Experiments .......................... 3-24

DSC Cooling Can .................................. 3-24Applications ....................................... 3-24Operation ............................................ 3-25

Quench-CoolingBetween Runs ................................. 3-25

Starting a Run BelowAmbient Temperature ..................... 3-26

Programmed Cooling ...................... 3-26


OverviewThis chapter gives step-by-step instructions onhow to run experiments with the 2010 instru-ment.

To obtain accurate results, follow the procedurescarefully, and check the calibration periodically(e.g., once a week).

Only the instructions necessary for runningexperiments are given in this chapter; explana-tions of terminology and how the instrumentoperates are given in Chapter 4, �TechnicalReference.�

Before You Begin

Before you set up an experiment, ensure that the2010 instrument, and the TA controller havebeen installed properly. Make sure you have:

� Made all necessary cable connectionsfrom the 2010 instrument to the TAcontroller

� Connected all gas lines� Powered up each unit (see Chapter 2)� Installed all appropriate options� Loaded the TA Operating System on the

controller� Become familiar with controller

operations� Calibrated the instrument, if necessary.

Overview

Running Experiments


Calibrating the DSCTo obtain accurate experimental results youshould calibrate the cell when you first installthe instrument. Once the initial calibrations aredone, you can save the resulting data files andreuse them when needed. For the best results,however, you should recalibrate periodically.

Perform calibration runs that encompass thetemperature range you plan to use in yourexperiments. If you change the general tempera-ture range of your experiments later, you maywish to recalibrate within the new range.

For precise experimental results you will need togenerate a new calibration file whenever youchange one of the following parameters:

� Ramp rate (selected in the thermal method)� Purge gas� Cooling technique (LNCA, RCS, or DSC

Cooling Can).

However, an acceptable alternative is to use aprevious calibration, if the conditions aresufficiently similar to those of the experimentsyou plan to run. Calibration is performed in theinstrument's calibration mode, which is accessedthrough the controller.

For more details on performing each type ofcalibration refer to the instructions in theThermal Solutions User Reference Guide.


Baseline Slope andOffset Calibration

This calibration involves heating an empty cellthrough the entire temperature range expected insubsequent experiments. The results may looksimilar to Figure 3.1. This figure shows twoexample heat flow curves for an empty standardDSC cell run from 25 to 400°C. Ideally, theheat flow signal should be zero, since there is nosample in the cell and it should have minimumslope. The calibration program is used tocalculate the slope and offset values needed toflatten the baseline and zero the heat flow signal.

Figure 3.1Baseline SlopeCalibration

Calibrating the DSC

Running Experiments


Cell ConstantCalibration

This calibration is based on a run in which acalibration material (e.g.,indium) is heatedthrough its melting point. The calculated heat offusion is compared to the theoretical value. Thecell constant is the ratio between these twovalues. The onset slope, or thermal resistance, isa measure of the temperature drop that occurs ina melting sample in relation to the themocouple.Theoretically, a calibration material should meltat a constant temperature. As it melts and drawsmore heat, a temperature difference developsbetween the sample and the sample thermo-couple. The thermal resistance between thesetwo points is calculated as the onset slope of theheat flow versus temperature curve on the frontof the melting peak. The onset value is used forkinetic and purity calculations to correct for thisthermal resistance.

TemperatureCalibration

Temperature calibration is based on a run inwhich a calibration material (e.g., indium) isheated through its melting point. The recordedmelting point of this material is compared to theknown melting point, and the difference iscalculated for temperature calibration. Thesame file used for the cell constant calibrationcan be used for this calibration.

In addition, you can use up to four other stan-dards to calibrate temperature. If you use onepair of known and observed points, the entirecurve is offset, or shifted, to the actual meltingpoint. If you use multiple standards, the tem-perature is corrected by a cubic spline fit. Themultiple-point temperature calibration is moreaccurate than the one-point calibration.


Running a DSC Experiment

Experimental Procedure

Your DSC experiments will have the followinggeneral outline:

� Selecting and preparing a sample. Thisinvolves preparing a sample of theappropriate size and weight, selectingthe pan type and material, andencapsulating the sample in the pan.

� Loading the sample pan (and a similarlyprepared empty reference pan) into thecell

� Entering experiment informationthrough the TA controller (sample andinstrument information)

� Creating and selecting the thermalmethod on the controller

� Attaching and setting up externalaccessories as required (e.g., purge gas,LNCA)

� Starting the experiment.


Running Experiments


Preparing Samples

Determining Sample Size

Normally, sample weight in DSC experiments isin the range of 5 to 20 milligrams. If puritydeterminations are to be performed, then samplesizes of 1 to 3 milligrams are recommended.Refer to Table 3.1 as a general guide for select-ing sample size and heating rates for yourexperiment.

Table 3.1DeterminingSample Size

Type of Sample Size HeatingMeasurement (mg) Rate

(oC/min)

glass 10 to 20 10 to 20transition (Tg)

melting point (Tm) 2 to 10 5 to 10

kinetics 5 to 10 5 to 20(Borchardt & Daniels)

kinetics (ASTM) * 0.5 to 20

heat capacity (Cp) 10 to 70 20

purity 1 to 3 0.5 to 1

crystallinity or 5 to 10 5 to 10oxidative stability

*Mass is inversely proportional to the heating rate.Use larger masses at slower rates, smaller massesat higher rates.


Physical Characteristics

When making quantitative measurements orverifying reproducibility, it is important toensure good thermal contact between the sampleand sample pan. The physical characteristics ofthe sample affect the quality of this contact.

When using powdered or granular samples,spread them evenly across the bottom of the panto minimize thermal gradients. For solidsamples, select the side of your sample with theflattest surface for contact with the pan. Afterencapsulating the sample, ensure that the panbottom is flat. If it is not, flatten it by pressingthe pan bottom on a flat surface.

The contact between the sample and sample panis as important as the contact between the panand the raised sample platform on the constantandisc.

Selecting Sample Pans

DSC samples must be in sample pans foranalysis. Use the following guidelines to selecta sample pan material and configuration thatmeets the temperature and pressure range,composition, and reactivity requirements of yourexperiment.

Sample Pan Material

Aluminum pans can be used in most experi-ments, unless the sample material reacts withaluminum or the temperature is expected to gobeyond that allowable for aluminum pans.Many other sample pan materials are availablefor experiments with special requirements. Forexample, you may wish to choose a particularpan material to improve the thermal conductanceto the sample.

NOTE:


Running Experiments


Sample pans made of platinum, copper, or goldare commonly used when the sample reacts withaluminum or has a transition in the 600 to 725oCregion; sample pans made of graphite are usedwhen alloying or other undesirable metal-sampleinteractions occur. The many pan materialsavailable enable you to study a wide variety ofsample materials over the temperature range ofthe DSC cell.

Table 3.2 provides guidelines for one of themost important factors in the selection of asample pan metal: the temperature range youplan to use in the experiment.

Table 3.2TA InstrumentsDSC Sample PanTemperature Ranges

Sample Pan UsableTemperatureRange (°C)

aluminum -180 to 600copper -180 to 725gold -180 to 725platinum -180 to 725graphite -180 to 725aluminum (SFI)* -180 to 600aluminum -180 to 600

[hermetic to 300 kPa(3 atm) internal pressure]

alodined aluminum -180 to 200[hermetic to 300 kPa(3 atm) internal pressure]

gold -180 to 725[hermetic to 600 kPa(6 atm) internal pressure]

*SFI = solid fat index



Sample Pan Configuration

Once you have selected the sample pan materialto be used, you must determine the appropriatesample pan configuration. Depending on therequirements of the experiment, samples can becontained in:

� Nonhermetic pans� Hermetic pans� Open pans (sample pans without lids).

Nonhermetic Pans

Most samples can be run in nonhermeticallycrimped aluminum sample pans. These pansprovide better thermal contact between sample,pan, and constantan disc than open pans;reduce thermal gradients in the sample; mini-mize sample spills; and enable you to retain thesample for further study.

Hermetic Pans

Hermetically sealed sample pans have the sameadvantages as the nonhermetic pans, plus theyhave an airtight seal that can resist higherinternal pressures (see Table 3.2). These pansare used for studies of: volatile liquids, mate-rials that sublime, aqueous solutions above100oC, and materials in a self-generated atmo-sphere. Because of its larger mass, a hermeticpan causes a slight loss of resolution comparedwith a nonhermetic pan; however, only thesystem time constant is affected, not thecalorimetric accuracy.

Running Experiments


Open Pans

Open pans (sample pans without lids) are usedwhen contact with the cell atmosphere orreaction of the sample with a gas is required.You can also use hermetic pans as open pans byputting a pinhole in the lid before sealing.

SFI Pans

SFI pans (so named because they were firstdeveloped for the solid fat index test) are idealfor waxy or oily substances. They contain aplatform on which the substance sits, whichprevents the substance from �wicking� up thesides of the pan. This maintains a constantsurface area during the experiment, which isespecially important in oxidative studies, inwhich increased surface area could result infaster oxidation.

Encapsulating the Sample

The Sample Encapsulating Press is used to sealboth nonhermetic and hermetic sample pans.Refer to Table 3.3 as a general guide for select-ing the encapsulating method for your experi-ment.



Table 3.3Selecting anEncapsulating Method

Sample Type Measurement Pan Type

solid Tg or Tm nonhermetic,(nonvolatile) oxidative hermetic,

stability SFI or openCp nonhermetic

solid (volatile) Cp hermetic

liquid crystal-lization hermetic,Tg or Tm SFI, or open

Cp hermetic

oxidative SFI or open

aqueous solution Cp, T

m, T

galodinedaluminumhermetic

Preparing Nonhermetic SamplePans

Before using the Sample Encapsulating Press,ensure that it is set up for nonhermetic crimping(see Appendix A).

Practice making a few nonhermetic sample pansto become familiar with this procedure beforeencapsulating your samples. If you have justchanged the die (from hermetic to nonhermetic),make a few sample pans to ensure that the diehas been installed properly.

Running Experiments


1. If you will be doing quantitative work,weigh the sample pan and lid.

When doing quantitative work, use tweezers tohandle the sample pan and lid. Touching themwith your fingers could leave residue that couldaffect your results.

2. Place the sample in the pan. If you are usinga powder or granular sample, spread itevenly in the pan.

3. Place a lid on the pan.

� If the sample is small or thin, powder,or granular, align the lid with the pan(see Figure 3.2).

� If the sample is large or bulky, invertthe lid and place it in the pan.

Pans used with inverted lids should not becrimped.

Figure 3.2Placing theCover Over the Pan

4. Place the sample pan in the well of thelower crimping die.

5. Pull the Sample Press lever forward until thehandle hits the stop.

6. Raise the lever and remove the pan withtweezers.

ALIGNED LID INVERTED LID

NON-HERMETIC PAN AND COVER

NOTE:

NOTE:


Figure 3.3NonhermeticallyCrimped Pans

7. Inspect the pan. The bottom of the panshould be smooth, and the sides shouldappear rolled down. If there is a ridge onthe bottom of the pan, loosen the lower dieholder thumbscrew and lower the bottom dieholder about ¼-turn by turning it clockwise,and repeat the process from step 4.


ALIGNED LID

SAMPLE

PAN BEFORECRIMPING

PAN AFTERCRIMPING

Running Experiments


Adjust the bottom die holder until you obtain aflat pan bottom. Then, lock the bottom dieholder in place by tightening the lower dieholder thumbscrew.

Large or bulky samples may rupture the pan lid. Ifthe lid ruptures, lower the bottom die holder.Slight deformation of the lid is acceptable.

8. For quantitative work, weigh the crimpedsample pan and lid (containing the sample)and determine the sample weight by sub-tracting the weight of the empty sample panand lid (step 1).

9. Prepare an empty nonhermetic pan and lid(follow steps 3 through 7) for use as thereference pan.

It is important that the same care be taken inpreparing the reference pan as in preparing thesample pan. The pan bottom should be flat.

Preparing Hermetic Sample Pans

Before using the Sample Encapsulating Press,ensure that it is set up for hermetic crimping (seeAppendix A).

Practice making a few hermetic sample pans tobecome familiar with this procedure beforeencapsulating your samples. If you have justchanged the die (from nonhermetic to hermetic),make a few hermetic sample pans to ensure thatthe die has been installed properly.

NOTE:

NOTE:


To prepare a hermetic sample pan:

1. For quantitative work, weigh the sample panand lid.

When doing quantitative work, use tweezers tohandle the sample pan and lid. Touching themwith your fingers could leave residue that couldaffect your results.

2. Carefully place the sample in the pan. Donot allow the sample to spill onto the lip ofthe pan. Put the hermetic lid on the pan, andplace the pan in the lower die in the SamplePress.

When using solid samples in hermetic pans forquantitative calorimetric measurements, invert thecover to improve sample-to-pan contact andminimize dead volume. This is especially importantfor purity analyses.

3. Place the flat side of the preforming toolagainst the upper die and hold it in place.With your other hand, pull the Sample Presslever forward until the preforming tool hitsthe stop.

4. Raise the lever and remove the preformingtool.

5. Lower the lever again with a steady motionuntil the handle hits the stop. Raise thelever and remove the pan with tweezers.

6. Inspect the pan. The bottom of the panshould be smooth, and there should be asmooth, complete seal around the circumfer-ence (as opposed to the rolled down appear-ance of a nonhermetic pan), indicating atight seal.


NOTE:

NOTE:

Running Experiments


7. For quantitative work, weigh the pan todetermine the sample weight.

8. Prepare an empty hermetic pan and lid foruse as the reference pan.

It is important that the same care be taken inpreparing the reference pan as in preparing thesample pan. The pan bottom should be flat.

NOTE:


Setting Up an Experiment

Setting Up Accessories

If your experiment requires additional accesso-ries, such as a purge gas or the LNCA, ensurethat they are turned on, and make any necessaryadjustments before you start your experiment.Ensure that the system can achieve the tempera-tures in all segments of the method (e.g., ifsubambient temperatures are required, makesure your cooling device is properly installedand filled). Use the following table as a guide inchecking your DSC accessories.

Table 3.4DSC AccessoryAdjustments

ExternalEquipment Check /Adjust:

Air cool Ensure that the air supplyline valve from the airsource is open.

Ensure that the pressure isbetween 20 and 120 psi.

Purge gas Make sure the correct gasis connected to the 2010instrument.

Ensure that your supply ofpurge gas is sufficient forthe needs of the experi-ment.

Set the purge gas flowrate.

(table continued)

Running Experiments



ExternalEquipment Check /Adjust:

LNCA Fill the LNCA tank withliquid nitrogen (see yourLNCA Operator�sManual).

Make sure the LNCA isconnected to the 2010instrument.

Turn on the LNCA.

Operation of the LNCA withthe 2010 instrument iscompletely automatic aslong as the power to theLNCA is on. The 2010 willoverride the LNCA controls,so there is no need to adjustthem.

Refrigerated Install the RCS CoolingCooling Head over the cell andSystem turn on the RCS.

Turn on the RCS andleave it on for 15 to 20minutes. Ensure thatsecond-stage cooling hasactivated before youbegin the run.

(table continued)

NOTE:



Table 3.4 (continued)

ExternalEquipment Check/Adjust:

DSC Install the DSCCooling Cooling Can over theCan cell and fill with the

desired coolant. Be readyto add more coolant asneeded during the experi-ment.

Gas Make sure the powerSwitching switch is on. Make sureAccessory the necessary gas

source(s) are properlyconnected.

Loading the Sample

Once the sample pan has been prepared and pre-experiment data has been recorded, you areready to load the sample pan into the DSC Cell.

If the cell has just been used, the compo-nents of the cell could be very hot. As asafe operating practice, use the tweezerswhenever handling the cell cover or silverlid.

Load the sample pan into the cell as follows:

1. Remove the bell jar, cell cover, and silverlid from the cell.

!WARNING

Running Experiments


2. Carefully place the sample pan on the frontraised platform and the reference pan on therear platform. Centering the pans within thegrid will ensure that they are centered on theplatforms (see Figure 3.4).

3. Replace the silver lid, cell cover, and belljar.

Figure 3.4DSC CellPan Positions


Starting an Experiment

Before you start the experiment, ensure that the2010 instrument is online with the controller andyou have entered all necessary experimentalparameters.

Start the experiment by pressing the START keyon the instrument keypad or Start from theThermal Solutions DSC Instrument Controlprogram, the instrument will run your method tocompletion.

Stopping an Experiment

If for some reason you need to discontinue theexperiment, you can stop it at any point bypressing either the STOP key on the 2010instrument keypad or choosing Stop on thecontroller. Another function that stops theexperiment is Reject on the controller. How-ever, the Reject function discards all of the datafrom the experiment; the Stop function savesany data collected up to the point at which theexperiment was stopped.

The REJECT function discards all experimentdata.


t CAUTION:

Running Experiments


Subambient ExperimentsSubambient experiments can be performed withthe DSC 2010 using the Liquid Nitrogen Cool-ing Accessory (LNCA), the Refrigerated Cool-ing System (RCS), and the DSC Cooling Can.Please consult the manuals that come with theLNCA and RCS for operation instructions.Instructions for operating the DSC Cooling Canare given below.

DSC Cooling Can

The DSC Cooling Can fits over the DSC Celland has a reservoir into which you can placecoolant to cool the cell. An open-top bell jar, aTeflon* disc, and a split O-ring are also includedwith the accessory.

Installation instructions for the DSC CoolingCan are given in Chapter 2.

ApplicationsThe DSC Cooling Can is used:

� To quench-cool (rapid-cool) betweenanalyses. The DSC Cell can be quench-cooled from 700°C to ambient in threeminutes.

� To cool to a subambient temperaturebefore a thermal program is started.

� To program-cool (by maintainingcoolant level in the reservoir).

* Teflon is a registered trademark of the DuPont Company.


Without the Teflon disc installed, the DSCCooling Can can be used over the entire tem-perature range of the DSC cell.

Operation

When the Teflon disc is installed, the DSC CoolingCan should not be placed on a hot cell withoutcoolant in the reservoir. Teflon softens at 325°C.

Quench-Cooling Between Runs

1. Carefully remove the DSC cell cover (it maybe hot). Place the DSC Cooling Can(without the Teflon disc) over the DSC Celland pour in the coolant, typically liquidnitrogen, using the open-top bell jar tominimize frost build-up on the can and DSCcell.

Follow the safety procedures in the front ofthis manual when handling liquid nitrogen.

2. When the cell cools to ambient, remove thebell jar and the DSC Cooling Can, and placethe sample and reference in the cell.

3. Replace the DSC Cooling Can if furthercooling is required.

To prevent frost from forming on the constantandisc, do not remove the silver lid when the celltemperature is below ambient.

Subambient Experiments

NOTE:

!WARNING

NOTE:

Running Experiments


Starting a Run Below Ambient Tem-perature

1. Place the sample and reference in the cell atambient temperature. Install the silver lidbut not the cell cover.

2. Place the DSC Cooling Can over the cell,and pour in the coolant using the open-topbell jar to minimize frost.

3. When the starting temperature is reached,remove the DSC Cooling Can, and place thecell cover and bell jar over the cell. Do notremove the silver lid.

Programmed Cooling

Once the Teflon disc is installed, you cannotremove it; the DSC Cooling Can will be set uppermanently for programmed cooling.

1. Place the sample and reference in the cell,and install the silver lid.

2. Place the Teflon disc in the DSC CoolingCan to minimize baseline disturbance whenthe can is refilled.

Teflon softens at 325°C. When the Teflon disc isinstalled, the DSC Cooling Can should not beplaced on a hot cell without coolant in the reser-voir.

3. Place the DSC Cooling Can and open-topbell jar over the cell, and pour in the cool-ant.

4. Start the programmed cooling. Add coolantas needed to keep the can at least half fullduring programmed cooling.

NOTE:

t CAUTION:


CHAPTER 4: Technical Reference

Description of the DSC 2010 ...................... 4-3

DSC Cell .................................................. 4-3

Principles of Operation ............................... 4-5

Cell Block Heating .................................. 4-5

Sample and Reference Thermocouples ... 4-6

DSC Applications ....................................... 4-7

Sample Types .......................................... 4-7

Status Codes ............................................... 4-8

Guidelines for Quantitative Studies .......... 4-12

Specific Heat Experiments ................. 4-12


Technical Reference


Description ofthe DSC 2010

A complete DSC 2010 system includes the 2010instrument and a controller. Both the tempera-tures and the heat flow associated with transi-tions in materials can be easily and rapidlymeasured by the system. The measurementsprovide quantitative and qualitative data relativeto physical or chemical changes of a materialinvolving endothermic (heat absorption) orexothermic (heat evolution) processes.

DSC CellThe DSC cell (Figure 4.1) uses a constantan(thermoelectric) disc as a primary heat-transferelement. A silver heating block, capped with avented silver lid, encloses the constantan disc.The selected sample and an inert reference areplaced in pans that sit on raised portions of thedisc. Heat is transferred through the constantandisc to both the sample and the reference pan.Differential heat flow to the sample and refer-ence are monitored by the CHROMEL®*-constantan area thermocouples formed at thejunctions of the constantan disc and theCHROMEL wafers welded to the underside ofthe two raised portions of the disc. CHROMELand ALUMEL®* wires are connected to theCHROMEL wafers at the thermocouple junc-tions to measure sample temperature. TheALUMEL wire welded to the reference wafer isfor thermal balance.

* CHROMEL® and ALUMEL® are registered trademarksof the Hoskins Manufacturing Company.

Description of the 2010


Technical Reference

Figure 4.1DSC Cell Cross-Section

Purge gas is preheated to heating block tempera-ture by circulation within the block beforeentering the sample chamber through the purgegas inlet. Gas exits through the vent hole in thesilver lid.

Vacuum and air cooling ports on the 2010instrument lead to openings in the cell but notdirectly to the sample chamber. A bell jar,placed over the cell and sealed with an O-ring,protects the operator from evolved gases andpermits cell evacuation.


Principlesof Operation

If a sample and an inert reference are heated at aknown rate in a controlled environment, theincrease in sample and reference temperaturewill be about the same (depending on specificheat differences), unless a heat-related changetakes place in the sample. If this change takesplace, the sample temperature either evolves orabsorbs heat). In DSC, the temperature differ-ence between sample and reference from such aheat change is directly related to the differentialheat flow.

Cell Block Heating

The 2010 instrument controls the cell tempera-ture by heating a silver block with a resistivewound heater and monitoring its temperaturewith a closely coupled control thermocouple.The appropriate amount of power supplied to theheater is determined by the difference betweenthe temperature measured by the control thermo-couple and the set point temperature (thetemperature the system is attempting to reach).

Heat from the block then flows radially throughthe constantan disc toward the sample andreference platforms. The primary means of heattransfer to the sample and reference is throughthe disc, although some heat is transferred fromthe lid and walls of the cell through the atmo-sphere.

The DSC cell uses Platinel II* control thermo-couples.

*Platinel II is a registered trademark of EnglehardIndustries.

Principles of Operation


Technical Reference

Sample andReference Thermocouples

The sample and reference thermocouples areconnected in series opposition (back-to-back) sothat if the sample (Ts) and reference (Tr) tem-peratures are the same, the resulting electricalpotential is zero. If the sample temperature ishigher than the reference, the output electricalpotential is one polarity; if the sample tempera-ture is lower, the polarity is reversed.

The DSC 2010 measures the differential voltagebetween the thermocouples at the sample andreference platforms. This voltage is linearized/converted to mW.

The sample platform (the front platform) alsohas an ALUMEL®* lead wire forming aCHROMEL®*-ALUMEL thermocouplejunction. The output from this thermocouple ismonitored on the T-axis after suitable coldjunction compensation. Thus, the signal isdetermined by CHROMEL-constantan thermo-couples, and the sample temperature is measuredwith a CHROMEL-ALUMEL thermocouple.The DSC cell baseline is very reproducible, andthe cell output can be compensated to obtain alevel baseline over the cell temperature rangewith the Thermal Solutions calibration func-tions.

* CHROMEL® and ALUMEL® are registered trademarksof the Hoskins Manufacturing Company.


DSC ApplicationsApplications of DSC fall into a broad categoryof materials characterization, including thermaltransitions in polymers:

� Glass transitions, crystallization, andmelting transitions

� Curing reactions and kinetics ofthermosets

� Oxidative stability of lubricants andpolymers

� Purity of pharmaceuticals and organics� Specific heat capacity of materials� Catalyst efficiency.

Sample Types

The 2010 instrument can be used to analyzevirtually any material that can be put into a DSCsample pan. The most important considerationis that the sample must make good thermalcontact with the pan. Samples of solids andliquids in any of the following forms can beanalyzed:

� Films� Fibers� Powders� Solutions� Composites.

DSC Applications


Technical Reference

Status CodesStatus codes are displayed at the top of theThermal Solutions Instrument Control window.

Table 4.1Method Status Codes

Code Meaning

Air Cool The cell is being aircooled by an Air Coolsegment or the Air CoolInstrument Controlfunction.

Autofill The LNCA is beingrefilled from a low-pressure bulk storagetank.

Calib The 2010 instrument isrunning in calibrationmode.

Cold The instrument heatercannot supply heat fastenough to keep up withthe thermal program. Thismay be caused by a largeballistic jump in theprogram, a faulty heater,or a faulty control thermo-couple signal.

(table continued)



Code Meaning

Complete The thermal method hasfinished.

Cooling The heater is cooling, asspecified by a Rampsegment.

Equilib The temperature is beingequilibrated to the desiredset point.

Heating The heater temperature isincreasing, as specified bya Ramp segment.

Holding Thermal experimentconditions are holding; theprogram is suspended.Choose Start to continuethe run.

Hot The temperature isbeyond the set point, andthe instrument cannotremove heat fast enoughto follow the thermalprogram. This is usuallycaused by a large ballisticjump to a lower tempera-ture or by a cooling rampbeing run without theLNCA.

(table continued)

Status Codes


Technical Reference


Code Meaning

Initial The temperature is beingequilibrated to the desiredset point. When thetemperature has reachedequilibrium, the status willchange to Ready.

Iso The thermal program isholding the currenttemperature isothermally.

Iso-track The instrument is holdingthe sample at a constanttemperature as specifiedby the Iso-track segment.

Jumping The heater is jumpingballistically to the set pointtemperature.

No Power No power is being mea-sured at the heater.Check the heater fuse.

Ready The system has equili-brated at the initialtemperature and is readyto begin the next segment.Choose Start to continuethe method.

Reject The experiment has beenterminated and the dataerased.

(table continued)


Status Codes


Code Meaning

Repeat The method is executing arepeat loop that does notinvolve temperaturecontrol segments.

Stand by The method and method-end operations arecomplete.

Temp The heater is in stand-bymode, and the experimenthas been terminated.


Technical Reference

Guidelines forQuantitative Studies

You can obtain DH and specific heat data fromDSC experiments by following the procedures inthis section. Optional heat capacity softwaregreatly simplifies these calculations.

Specific HeatExperiments

If you wish to calculate specific heat, follow theguidelines below when running the sample.

1. Create a baseline profile:

a. Load the cell with empty sample andreference pans. Include lids if yourexperiment will use sealed pans, but donot crimp the sample pan (you will needto reuse it).

b. Create a method that holds isothermallyat the desired starting temperature for 5minutes, heats at the desired heat rate,and then holds at the limit temperaturefor 2 minutes.

c. Start the run. Deflection from the initialequilibrium point may be upward ordownward, depending on the specificheat difference between the sample andreference pans.


2. Repeat the run under identical conditionswith a weighed sample in the same samplepan used for the baseline profile. Do notadjust the baseline slope or use the AutoZero A or Manual Zero A option betweenthe runs.

3. Plot the above thermograms with the dataanalysis program. Use the same limits andintervals in both plots.

4. Calculate the specific heat by measuring thedifference in y-axis displacement (calori-metric differential) between the sample andblank curves at any desired temperature (seeFigure 4.2).

Figure 4.2Specific Heatof Sapphire

5. Substitute the difference into the followingequation:

Guidelines for Quantitative Studies

DH = 18.5 mW

E = Cp Hr m 60 DH

DH mCp =

60 E Hr

DH = 23.5 mW


Technical Reference

where E = cell calibration coefficient at thetemperature of interest(dimensionless)

Hr = heating rate, in oC/minute

DH = difference in y-axis deflectionbetween sample and blankcurves at the temperature ofinterest, in mW

m = sample mass, in mg

Cp = specific heat, in J/goC

The quantity 60E /Hr is constant under a givenset of experimental conditions. It converts the ymeasurement directly into units of specific heatin J/goC. For greatest accuracy, determine thevalue of this constant (as an entity) by running astandard material of known specific heat underconditions identical to those of the unknownsample. Then substitute the values of H, m, andCp for the standard into the above equation at thetemperature of interest.

A sapphire (Al2O3) standard is provided in theaccessory kit for this purpose. Table 4.4 (pages4-15 to 4-18) shows its respective specific heatvalues.

The values in the table were determined byGinnings and Furukawa of the National Bureauof Standards on aluminum oxide in the form ofsynthetic sapphire (corundum). The sapphirepieces passed a #10 sieve but were retained by a#40 sieve, and had 99.98 to 99.99 percent purityby weight. Specific heat values below theexperimental range were obtained by extrapola-tion of a Debye equation fitted to the ex-perimental value at the lowest temperature.



Cp

Table 4.2Aluminum OxideSpecific Heat*

°C K J/g°C

-183.15 90 0.0949-173.15 100 0.1261-163.15 110 0.1603-153.15 120 0.1968-143.15 130 0.2349-133.15 140 0.2739-123.15 150 0.3134-113.15 160 0.3526-103.15 170 0.3913 -93.15 180 0.4291 -83.15 190 0.4659 -73.15 200 0.5014 -63.15 210 0.5356 -53.15 220 0.5684 -43.15 230 0.5996 -33.15 240 0.6294 -23.15 250 0.6579 -13.15 260 0.6848 -3.15 270 0.7103 0.00 273.15 0.7180 6.85 280 0.7343 16.85 290 0.7572 26.85 300 0.7788 36.85 310 0.7994 46.85 320 0.8188 56.85 330 0.8373 66.85 340 0.8548

*Taken from D.A. Ditmars, et.als.,J. Res. Nat.Bur. Stand., Vol 87, No. 2,pages 159-163 (1982). This is a publicdomain publication.

(table continued )


Technical Reference

Cp

Table 4.2 (continued)*

°C K J/g°C

76.85 350 0.8713 86.85 360 0.8871 96.85 370 0.9020106.85 380 0.9161116.85 390 0.9296126.85 400 0.9423136.85 410 0.9545146.85 420 0.9660156.85 430 0.9770166.85 440 0.9875176.85 450 0.9975186.85 460 1.0070196.85 470 1.0161206.85 480 1.0247216.85 490 1.0330226.85 500 1.0409236.85 510 1.0484246.85 520 1.0557256.85 530 1.0627266.85 540 1.0692276.85 550 1.0756286.85 560 1.0817296.85 570 1.0876306.85 580 1.0932316.85 590 1.0987326.85 600 1.1038336.85 610 1.1089

*Taken from D.A. Ditmars, et.als., J. Res.Nat.Bur. Stand., Vol 87, No. 2, pages 159-163(1982). This is a public domain publication.

(table continued )



Cp


°C K J/g°C

346.85 620 1.1137356.85 630 1.1183366.85 640 1.1228376.85 650 1.1271386.85 660 1.1313396.85 670 1.1353406.85 680 1.1393416.85 690 1.1431426.85 700 1.1467446.85 720 1.1538466.85 740 1.1604486.85 760 1.1667506.85 780 1.1726526.85 800 1.1783546.85 820 1.1837566.85 840 1.1888586.85 860 1.1937606.85 880 1.1985626.85 900 1.2030646.85 920 1.2074666.85 940 1.2117686.85 960 1.2159706.85 980 1.2198726.85 1000 1.2237746.85 1020 1.2275766.85 1040 1.2312786.85 1060 1.2348

*Taken from D.A. Ditmars, et.als., J. Res.Nat.Bur. Stand., Vol 87, No. 2, pages 159-163(1982). This is a public domain publication.

(table continued )


Technical Reference


°C K J/g°C

806.85 1080 1.2383826.85 1100 1.2417846.85 1120 1.2451866.85 1140 1.2484886.85 1160 1.2516906.85 1180 1.2548926.85 1200 1.2578976.85 1250 1.26531026.85 1300 1.27241076.85 1350 1.27921126.85 1400 1.28561176.85 1450 1.29171226.85 1500 1.29751276.85 1550 1.30281326.85 1600 1.30791376.85 1650 1.3128

*Taken from D.A. Ditmars, et. als., J. Res.Nat.Bur. Stand., Vol 87, No.2, pages 159-163(1982). This is a public domain publication.

Cp


CHAPTER 5: Maintenance andDiagnostics

Overview ..................................................... 5-3

Routine Maintenance .................................. 5-4

Inspection ................................................ 5-4

Cleaning the Instrument Keypad ............. 5-4

Cleaning a Contaminated Cell ................. 5-4

Sample Encapsulating Press .................... 5-7

Diagnosing Power Problems ....................... 5-8

Fuses ........................................................ 5-8

Power Failures ......................................... 5-9

DSC 2010 Test Functions ......................... 5-12

2010 Confidence Test ............................ 5-12

Replacement Parts .................................... 5-13

Maintenance and Diagnostics



OverviewThe procedures described in this section are thecustomer�s responsibility. Any further main-tenance should be performed by a representativeof TA Instruments or other qualified servicepersonnel.

Because of the high voltages in this instru-ment, untrained personnel must not at-tempt to test or repair any electricalcircuits.

!WARNING

Overview



Routine Maintenance

InspectionExamine the instrument periodically for goodcondition. Ensure that the furnace area is clean.Any sample spillage or residue should beremoved before the next experiment.

Cleaning theInstrument Keypad

You can clean the 2010 instrument keypad asoften as you like. The keypad is covered with asilk-screened Mylar* overlay that is reasonablywater resistant but not waterproof or resistant tostrong solvents or abrasives.

A household liquid glass cleaner and papertowel are best for cleaning the instrumentkeypad. Wet the towel, not the keypad, with theglass cleaner, and then wipe off the keypad.

Cleaning aContaminated Cell

A poor baseline is often the sign of a contami-nated cell. The cell must be cleaned properly tomaintain satisfactory operation. Scraping thecontamination off is not recommended becausethe constantan disc is very thin (about 0.1 mm,or 0.004 inches), and if the disc deforms, thebaseline may be affected. Scraping can causesevere damage to the cell if it is not donecarefully.

* Mylar is a registered trademark of the DuPontCompany.


If your baseline performance begins to deterio-rate, try the following recommended cleaningprocedure.

Begin cleaning by heating the cell with an airpurge to 50°C above your normal upper tem-perature or 600°C, whichever is lower, withoutpans or bell jar. Use a heating rate of 20°C perminute. After cool-back to room temperature,lightly brush out the cell with a small fiberglasseraser (included in the DSC accessory kit), runthe method again, and compare the baselines. Ifthere is a marked improvement but the baselineis still unacceptable, the contaminant probablyoxidized and reduced to an inert ash. Run themethod again and check for further improve-ment. Once the baseline is acceptable, return tonormal operation.

If the constantan disc looks clean and is not bentor cracked, but the baseline problem remains, itis probably not due to contamination; the cellmay need to be replaced (contact your TAInstruments service representative).

Cleaning DSC Pans

The aluminum, gold, and copper pans and thehigh pressure capsules provided for use with TAInstruments DSC systems are manufactured tohigh quality standards, including cleaning toremove contaminants that might be present fromthe manufacturing process. For most applica-tions, these pans can be used as received;however, if the pans are used for high sensitivityexperiments (e.g., oxidative stability), anadditional cleaning process is recommendedbefore use. This procedure is taken from

Routine Maintenance



Appendix A of ASTM standard E1858 TestMethod for Oxidative Induction Time of Hydro-carbons by Differential Scanning Calorimeters.

Follow the steps below to clean the TA Instru-ments DSC sample pans:

1. Place 200 pans in a 250 mL Erlenmeyerflask that has been fitted with a glassstopper.

2. Add approximately 150 mL of reagent gradexylene (enough to cover the pans).

3. Swirl the flask, containing the pans andxylene, for 0.5 to 2.0 min.

4. Let the flask stand for 1.0 min.

5. Decant the xylene out of the flask.

6. Repeat steps 1 through 5.

7. Add approximately 150 mL of reagent gradeacetone after the second xylene wash.

8. Swirl the flask, containing the pans andacetone, for 0.5 to 2.0 min.

9. Let the flask stand for 1.0 min.

10. Decant the acetone out of the flask.

11. Repeat steps 7 through 10.

12. Rotate the flask�so that no pans adhere tothe bottom or side of the flask�as you flownitrogen at 150 to 200 mL/min over the wetpans to drive off the excess solvent. Thisshould take approximately 5 to 6 min.


13. Return the cleaned pans to their storagecontainer and record the date they werecleaned.

SampleEncapsulating Press

The only maintenance needed for the SampleEncapsulating Press is an occasional drop oflight machine oil on the cam. Also, make surethe dies are free of material that could scratchtheir surfaces and impair the seal.

Routine Maintenance



Diagnosing Power Problems

FusesThe 2010 instrument contains several internalfuses; however, they are not user serviceable. Ifany of the internal fuses blow, a hazard mayexist. Call your TA Instruments service repre-sentative.

The only fuses that you should service yourselfare the external fuses, located on theinstrument's rear panel. Both slo-blo type fusesare housed in safety-approved fuse carriers,labeled F1 and F2 (see Figure 5.1).

Figure 5.1Fuse Locations

Always unplug the instrument before youexamine or replace the fuses.

FUSE

FUSE

Fuse 1

Fuse 2

!WARNING

10 A


Fuse F1 is in the circuit between the mainelectrical input and the low power loads. Allpower for internal operations and instrumentfunctions, except heater power and solenoidvalves, passes through this fuse. If this fuseblows, you will get no response from the instru-ment when you attempt to turn it on.

Fuse F2 protects the heater coils in the furnaceand supplies power to the optional LNCA.Because fuse F2 does not power the internallogic, you may not know that this fuse is blownuntil you try to heat a sample; the 2010 passesthe confidence test with this fuse open.

Fuse F2 is always checked at the beginning of amethod. Power supplied by this circuit isswitched by a computer-controlled relay. If fuseF2 is open at the start of a run, then Error 73�No heater power at method start� is displayedand the run is terminated.

Power Failures

A power failure caused by a temporary drop inline voltage results in one of two responses bythe DSC 2010 instrument:

� If the drop is fairly large and of longduration (20 milliseconds or more), thesystem will reset and go into its power-up sequence when power resumes.

� If the drop is small or of short duration,the system may halt. The instrument willnot restart until reset. To reset, pressthe Reset button on the 2010 instrumentback panel.

Diagnosing Power Problems



The 2010 instrument is designed for a nominalline voltage of 115 volts AC (± 10%), 50 or 60Hz. It should not be operated outside this range.Low line voltage may result in poor instrumentoperation; high line voltage may damage theinstrument.


DSC 2010 Test FunctionsThe DSC 2010 has three levels of test anddiagnostic functions:

� The confidence test that is run every timethe instrument is started.

� Cycling test functions that continuously testspecific.

� A manufacturing verifier test mode thatcoordinates and logs the results of asequence of confidence test and drift runs.

These test functions are always present in theinstrument. They are designed to aid manufac-turing and service in checking and repairing theinstrument.

The Confidence Test

Every time the 2010 instrument is powered up orreset, it automatically performs an internalconfidence test of the instrument electronics.The confidence test takes approximately 16seconds to complete. During the confidence testthe yellow ready light on the front and rear ofthe instrument will flash several times, indicat-ing that the test is proceeding normally.

If the confidence test is completed withoutany fatal errors detected, then the ready lightwill turn on and remain on steadily, and theinstrument will sound a beep. The instrumentis now ready to be configured online with thecontroller.

DSC 2010 Test Functions



If a fatal problem is detected during the confi-dence test, then the ready light will remain off,or continue to flash periodically. The instru-ment cannot be configured online when fatalerrors are detected. Contact your TA Instru-ments service representative for assistance.

If the confidence test detects a non-fatal problemduring start-up, a confidence test error messagewill be displayed on the controller when theinstrument is configured online. Non-fatal error15, �CMOS RAM checksum error,� is displayedimmediately after new instrument software isloaded into the 2010 instrument. Resetting theinstrument should clear this error. If error 15persists, or if any other confidence test errors aredisplayed, contact your TA Instruments servicerepresentative for assistance.


Replacement Parts

Replacement PartsTable 5.1List of DSC2010 Parts

Part Number Description

900155.000 bell jar, glass dome top forDSC Cell

900681.002 bell jar, glass open top forDSC Cooling Can

900660.903 DSC accessory kit910824.001 DSC cleaning brush900639.901 DSC cover925604.001 DSC 2010 Operator�s

Manual983045.901 event cable205220.021 fuse, 1.25 amp ceramic205220.040 fuse, 10.00 amp ceramic202814.339 O-ring, Neoprene, for bell

jar900682.001 O-ring, Silicon, split for

DSC Cooling Can900786.901 pan bottoms, aluminum

crimp900779.901 pan covers, aluminum

crimp253827.000 power cable, 110 V900635.000 silver lid for DSC, flat

with hole259538.000 stainless steel needle-point

tweezer202515.000 standard, sapphire specific

heat900902.901 standard, vial of indium

metal

(table continued)



Table 5.1List of DSC2010 Parts(continued)

Part Number Description

993003.001 DSC 2010/TGA 2050Service Manual

900578.901 Sample pans, platinum900786.901 Sample pans, aluminum900779.901 Sample pan lids, aluminum900793.901 Sample pans, aluminum,

hermetic900794.901 Sample pan lids, alumi-

num, hermetic900860.901 Sample pan lids, alumi-

num, hermetic with pinhold

900796.901 Sample pans, coatedaluminum, hermetic

900790.901 Sample pan lids, coatedaluminum, hermetic

900870.901 Sample pans, aluminum,for SFI samples

900866.901 Sample pans, gold900868.901 Sample pan lids, gold900871.901 Sample pans, gold,

hermetic900872.901 Sample pan lids, gold,

hermetic900867.901 Sample pans, copper900869.901 Sample pan lids, copper900874.901 Sample pans, graphite900873.901 Sample pan lids, graphite

TA INSTRUMENTS DSC 2010 A–1

The Sample Enclapsulating Press

Appendix A: The SampleEncapsulating Press

Introduction

The Sample Encapsulating Press is used to sealsamples in hermetic and nonhermetic samplepans. Two dies come with the press: one forhermetic sealing and one for nonhermeticsealing. This appendix explains how to changethese dies.

Instructions for sealing samples with the SampleEncapsulating Press are given in Chapter 3 ofthis manual.

Figure A.1Sample Encapsulating PressWith Nonhermetic Dies Installed

Appendix A

A–2 TA INSTRUMENTS DSC 2010

Setting Up the Pressfor Nonhermetic Sealing

The Sample Encapsulating Press is shipped withthe upper nonhermetic die installed. To set upthe press to make nonhermetic sample pans(when the die is set up for hermetic pans),proceed as follows:

l. Remove the hermetic die set:

a. Loosen the thumbscrew on the columnof the Sample Press (see Figure A.1).

b. Lower the lower die holder by turningthe base screw on the bottom of thepress counterclockwise.

Figure A.2Lowering the Base Screw

c. Lift the lower hermetic die and removeit from the die holder.



2. Place the lower nonhermetic die (FigureA.3) into the lower die holder (large endup).

Figure A.3The Nonhermetic Dies

3. Place the upper nonhermetic die around theplunger of the upper hermetic die (visiblewhen the lever is lowered).

4. Push the upper nonhermetic die upwardagainst the spring-loaded plunger and lock itin place by tightening the setscrew (FigureA.4) with a 0.050" hex wrench.

SETSCREW

Appendix A


Figure A.4Lower Die Setscrew

5. Adjust the height of the upper and lowerdies:

a. Pull the Sample Press lever all the waydown (until it rests on the column).

b. Turn the screw on the underside of thepress clockwise as far as it will go.Then turn the screw back about ¼ turnand tighten the lower die holder thumb-screw to lock the lower die holder inplace. When the press is adjustedproperly, the upper and lower dies justtouch. The height of the bottom die mayneed adjusting based on the sampleheight.

LOWER DIESETSCREW



c. Make a few sample pans (see Chapter 3)to check the die setting. A good nonher-metic pan will have a flat bottom, andthe sides of the pan will appear rolleddown (see Table A.1).

Table A.1Specifications for Nonhermetic Pans

Uniform foldingof lid aroundcircumference

Flat surfaceon the bottomof the pan; noridge aroundcircumference

No visible gapsbetweenlid and pan

Appendix A


Setting Upthe Press forHermetic Pans

l. Remove the nonhermetic die set:

a. Lower the lever until you can see thesetscrew on the upper nonhermetic die.If necessary, turn the upper die to accessthe lower die setscrew. Loosen thesetscrew (Figure A.4) with a 0.050" hexwrench, raise the lever, and remove theupper die.

b. Loosen the thumbscrew on the columnof the Sample Press (see Figure A.1).

c. Lift the lower nonhermetic die andremove it from the die holder.

2. Place the lower hermetic die (Figure A.5)into the lower die holder, either end up.

Figure A.5The Hermetic Dies



3. Check the spring tension of the upperhermetic die (this is the die that remains inthe press when the nonhermetic die isremoved) by pushing up on the centerplunger. If the plunger does not move,adjust the spring tension as follows:

a. Lower the Sample Press lever. Raisethe lower die holder until it contacts theupper die holder, then unscrew theholder ¼ turn. (Loosen the thumb-screw before unscrewing the lower dieholder.)

b. Keep the lever down and unscrew theupper die setscrew, letting the die comein contact with the lower die. (Theupper die is spring loaded and will snapdown to contact the lower die.)

c. Tighten the setscrew on the upper die.

d. Check the tension again. Continue toadjust until you can move the upper dieplunger.

4. Adjust the setting of the upper and lowerdies:

a. Pull the lever down all the way (until itrests on the column).

b. Turn the screw on the underside of thepress clockwise as far as it will go.Then turn the screw back about ¼-turnand tighten the lower die holder thumb-screw to lock the lower die holder inplace.

Appendix A


c. Make a few sample pans to check thedie setting (see Chapter 3 for instruc-tions). A good hermetic pan will have aflat bottom, with a complete seal aroundthe circumference of the pan, and thesides of the pan will appear flat andsmooth (see Figure A.6).

Figure A.6Properly SealedHermetic Pan

TA INSTRUMENTS DSC 2010 B–1

Appendix B: Ordering Information

TA Instruments, Inc.109 Lukens DriveNew Castle, DE 19720Telephone: 1-302-427-4000 or 1-302-427-4040Fax: 1-302-427-4001

HELPLINE�U.S.A.For technical assistance with current orpotential thermal analysis applications,please call the Thermal Analysis Help Deskat 1-302-427-4070.

SERVICE�U.S.A.For instrument service and repairs,please call 1-302-427-4050.

TA Instruments Ltd.Europe House, Bilton CentreCleeve RoadLeatherhead, Surrey KT22 7UQEnglandTelephone: 44-1372-360363Fax: 44-1372-360135

TA Instruments GmbHMax-Planck-Strasse 11D-63755 AlzenauGermanyTelephone: 49-6023-9647-0Fax: 49-6023-9647-77

TA Instruments BeneluxOttergemsesteenweg 461B-9000 GentBelgiumTelephone: 32-9-220-79-89Fax: 32-9-220-83-21

Appendix B

B–2 TA INSTRUMENTS DSC 2010

TA Instruments JapanNo. 5 Koike Bldg.1-3-12 KitashinagawaShinagawa-Ku, Tokyo 140JapanTelephone: 813/3450-0981Fax: 813/3450-1322

TA Instruments FranceB.P. 60878056 Saint-Quentin-YvelinesCedexFranceTelephone: 33-1-30-48 94 60Fax: 33-1-30-48 94 51

TA Instruments SpainWaters Cromatografía, S.A.División TA InstrumentsAvda. Europa, 21. Pta. Baja28108 AlcobendasMadrid, SpainTelephone: 34-91-661-8448Fax: 34-91-661-0855

TA Instruments AustraliaUnit 338-46 South StreetRydalmere NSW 2116AutstraliaTelephone: 61-29-9331-705Fax: 61-29-8981-455

TA Instruments ItalyDivision of Waters SpAvia Achille Grandi 2720090 Vimodrone (MI), ItalyTelephone: 39-02-27421-1Fax: 39-02-250-1827

Printed in U.S.A.

TA INSTRUMENTS DSC 2010 I–1

Index

Index

A

accessories 1-6Cooling Can 1-13LNCA 1-11setting up 3-19subambient 1-11

address 2-10

applications 4-7

C

cablesconnecting 2-9

cellcleaning 5-4description 1-9unpacking 2-6

cell blockheating 4-5

cleaning 5-4DSC pans 5-5

Complete (status code) 4-9

components 1-5

constantan disc 4-5

Cooling (status code) 4-9

Cooling Can 3-24installation 2-17�2-21operation 3-25�3-26

D

DSC 2010accessories 1-6, 1-10applications 4-7cleaning 5-4

pans 5-5connecting cables 2-9connecting gas lines 2-9connector panel 2-10cross-section 4-4description 1-3function 1-4inspection 2-7keypad 1-7lines 2-12location of 2-8maintenance 5-4power cable 2-15power problems

failures 5-7fuses 5-6

power switch 1-9repacking 2-6replacement parts 5-11shutting down 2-21specifications 1-14�1-16starting 2-20unpacking 2-3

I–2 TA INSTRUMENTS DSC 2010

Index

E

Equilib (status code) 4-9

experimentprocedure 3-7�3-26running 3-7�3-26starting 3-23�3-26stopping 3-23subambient 3-24

starting 3-26

F

fuses 5-6

G

gaspurge 1-15

Gas Line 2-13

gas linesconnecting 2-9

GPIB Cableconnecting 2-9

H

Heat Capacity 4-12

Heating (status code) 4-9

hermetic panspreparing 3-16

Holding (status code) 4-9

Hot (status code) 4-9

I

Initial (status code) 4-9

Iso (status code) 4-9

K

keypad 1-7

L

lights 2-20�2-21

LNCA 1-11

N

nonhermetic panspreparing 3-13

P

powerproblems with fuses 5-6

power cable 2-15

POWER light 2-20

problemspower problems 5-6

programmed cooling 3-26

TA INSTRUMENTS DSC 2010 I–3

Index

purge gases 1-15

Purge Line 2-12

R

READY light 2-20, 5-10

routine maintenance 5-4

S

samplecharacteristics 3-9encapsulating 3-12

Sample Encapsulating Pressmaintenance 5-5

sample panshermetic 3-11nonhermetic 3-11open 3-12

sample size 3-8

samplespreparing 3-8types 4-7

shutting down 2-21

specifications 1-14

Stand by (status code) 4-11

Start Upof DSC 2010 2-20

Status Codes. See also name ofstatus code

list of 4-8

subambient operationCooling Can installation 2-17installations for 2-16

systemturning off 2-21

T

Temp (status code) 4-11

thermocouplesdescription 4-6

U

unpacking 2-3

V

vacuum line 2-13

I–4 TA INSTRUMENTS DSC 2010

Index

dsc2010 user manual

Documents

iiita instruments dsc

dsc cooling

dsc cell

introducingthe dsc

instrument keypad

cooling gas lines

e text onlyissued

data analysis