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TA DISCOVERY DSC2500 Getting Started Manual

Differential scanning calorimeter
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DISCOVERY DSC™
DIFFERENTIAL SCANNING CALORIMETER
Getting Started Guide for
DSC2500, DSC250, DSC25
Revision C
Issued December 2016

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Summary of Contents for TA DISCOVERY DSC2500

  • Page 1 DISCOVERY DSC™ DIFFERENTIAL SCANNING CALORIMETER Getting Started Guide for DSC2500, DSC250, DSC25 Revision C Issued December 2016...
  • Page 2 TA Instruments may have patents, patent applications, trademarks, copyrights, or other intellectual prop- erty covering subject matter in this document. Except as expressly provided in written license agreement from TA Instruments, the furnishing of this document does not give you any license to these patents, trademarks, copyrights, or other intellectual property.

  • Page 3: Introduction

    Introduction Important: TA Instruments Manual Supplement Please click the TA Manual Supplement link to access the following important information supplemental to this Getting Started Guide: • TA Instruments Trademarks • TA Instruments Patents • Other Trademarks • TA Instruments End-User License Agreement •...

  • Page 4: Notes, Cautions, And Warnings

    Notes, Cautions, and Warnings This manual uses NOTES, CAUTIONS, and WARNINGS to emphasize important and critical instructions. In the body of the manual these may be found in the shaded box on the outside of the page. NOTE: A NOTE highlights important information about equipment or procedures. CAUTION: A CAUTION emphasizes a procedure that may damage equipment or cause loss of data if not followed correctly.

  • Page 5: Electromagnetic Compatibility Standards

    Electromagnetic Compatibility Standards For the United States CFR Title 47 Telecommunication Chapter I Federal Communications Commission, Part 15 Radio frequency devices (FCC regulation pertaining to radio frequency emissions). CAUTION: This equipment is not intended for use in residential environments and may not provide adequate protection to radio reception in such environments.

  • Page 6: Safety

    If you are not trained in electrical procedures, do not remove the cabinet covers unless specifically instructed to do so in the manual. Maintenance and repair of internal parts must be performed only by TA Instruments or other qualified service personnel.

  • Page 7: Electrical Safety

    120/240 VAC are present in the instrument. DANGER: Risk of electric shock. High voltages are present in this instrument. Maintenance and repair of internal parts must be performed only by TA Instruments or other qualified service per- sonnel. DANGER: Risque de choc électrique. Présence de tensions élevées dans cet instrument. La maintenance et la réparation des pièces internes doivent être effectuées uniquement par TA...

  • Page 8: Thermal Safety

    Thermal Safety DANGER: The cell surfaces can be hot enough to burn the skin during a sample run. If you are conducting a subambient test on the DSC, cold could also cause injury. After running any type of experiment, you must allow the DSC cell to return to room temperature before you touch the inner cell surfaces.

  • Page 9: Laser Safety

    Laser Safety This instrument is a Class 1 Laser product. Do not stare into the beam. Exempt laser product. Class 1 Laser Products are accompanied by the following label: This product complies with IEC 60825-1, with FDA performance standards for laser products. 21 CRF 1040.10 except for deviation pursuant to Laser Notice No.50.

  • Page 10: Table Of Contents

    Table of Contents Introduction ..............................2 Important: TA Instruments Manual Supplement ................... 2 Notes, Cautions, and Warnings ......................3 Regulatory Compliance .......................... 3 Safety Standards ..........................3 Electromagnetic Compatibility Standards ....................4 Safety ..............................5 Instrument Symbols ......................... 5 Electrical Safety ..........................6 Handling Liquid Nitrogen .......................
  • Page 11 Use, Maintenance, & Diagnostics ......................51 Using the Discovery DSC™........................51 Before You Begin ..........................51 Calibrating the Discovery DSC™ ......................52 T1 Baseline Calibration (Discovery DSC2500, DSC250, DSC25) ............. 52 ® Tzero Calibration ..........................52 Enthalpy (Cell) Constant Calibration ....................53 Temperature Calibration ........................

  • Page 12: Introducing The Discovery Dsc™ 2500, Dsc250, Dsc25

    It can also be used to measure and quantify the heat capacity of a material. This information helps the scientist or engineer identify processing and end-use performance. Figure 1 Discovery DSC2500 shown. Your controller is a computer that performs the following functions: •...

  • Page 13: Dsc System Components

    DSC System Components A functional Discovery DSC™ system has two major components: the Discovery DSC instrument, which includes the DSC cell used for monitoring differential heat flow and temperature and a gas delivery mod- ule; and a cooling accessory. The cooling accessory selected depends on the temperature range desired for your experiments.
  • Page 14 This simple relationship, however, does not take into account extraneous heat flow within the sensor. The TA Instruments DSC is specifically designed to account for those latter heat flows. The cell sensor consists of a constantan transducer with separate chromel disk welded to the surface under the sample platform.

  • Page 15: Gas Delivery Module

    It also measures the base purge flow, which prevents frosting when cooling accessories are used, and switches on/off the cooling gas flow. DSC Autosampler The Autosampler (shown below) is standard on the TA Instruments Discovery DSC2500, and optional for the Discovery DSC25 and DSC250. Figure 3 Discovery DSC2500 with Autosampler.

  • Page 16: Finned Air Cooling System (Facs)

    Finned Air Cooling System (FACS) The Finned Air Cooling System (FACS) allows operation from ambient to 725°C, using flowing air as the coolant. For installation instructions, see Chapter 2. You can use the optional Quench Cool accessory with the FACS (see next section) if you want to return the temperature of the cell to ambient more quickly. This cooler is not intended for use at temperatures below ambient due to the potential for frost formation on the fins.

  • Page 17: Refrigerated Cooling System (Rcs)

    The Refrigerated Cooling Systems (RCS) are used to perform DSC cooling experiments. There are three different models offered by TA Instruments: the new RCS120, the RCS90, and the RCS40. All three mod- els have a cooling head, which is made up of an internal heat exchanger, anti-condensate heaters, and vari- ous other components.

  • Page 18: Liquid Nitrogen Pump (Ln Pump)

    Liquid Nitrogen Pump (LN Pump) The Liquid Nitrogen Pump (LN Pump) is a cooling accessory that allows continuous temperature control within the range of –180 to 550°C. The LN Pump delivers (via a pump) liquid nitrogen to the heat exchanger, which in turn cools the cell. The LN Pump can be controlled from the General panel of TRIOS software or the user interface on Dis- covery DSC 25, DSC 250, and DSC 2500 units.

  • Page 19: The Discovery Dsc™ User Interface

    The Discovery DSC™ User Interface The Discovery DSC includes an integrated user interface display for local operator control. The functions of the user interface change depending upon the view displayed. This section briefly describes the basic layout of these functions. Status line View panel Primary function buttons...

  • Page 20: Primary Function Buttons

    Primary Function Buttons Use the following buttons for the main functions of the instrument. Table 1: Primary Function Buttons on the User Interface Key Name Description Start Begins the currently-programmed experiment. This is the same function as Start on the instrument control software. Start automatically loads the selected sample pan and closes the furnace, if necessary, before beginning the experiment.

  • Page 21: View Panel

    View Panel The view panel provides real-time instrument status and additional functionality pertinent to the selected operation. A list of available functions is described below. Table 2: View Panel Functions on the User Interface Button Name Description System Info Displays instrument information such as the serial number, IP configu- ration, and network configuration.

  • Page 22: Additional Function Buttons

    Additional Function Buttons Button Name Description Help The Help button can be found on the lower right side of some screens, and displays information regarding use of the currently displayed touch- screen. Autosampler Stop Displayed while the Autosampler is in motion, pressing this button will stop the Autosampler, and can be used instead of the Stop button.

  • Page 23: Instrument Specifications

    Instrument Specifications The tables found below contain the technical specifications for the Discovery DSC™ Table 3: Discovery DSC Technical Specifications Item/Area Specifications Dimensions Depth 51 cm (20 in) Width 53 cm (21 in) Height 53 cm (21 in) Weight (with Autosampler and FACS) 32 kg (70 lbs) Mains Power 100–240 VAC, 50/60 Hz, 600 W...
  • Page 24 CAUTION: Holding the Discovery DSC™ cell at high temperatures for extended periods of time may cause sticking of the silver lid. If this occurs, please contact TA Instruments for assistance in removing the lid.

  • Page 25: Options And Accessories

    Options and Accessories Several additional pieces of equipment are available from TA Instruments to be used with the Discovery DSC™. A brief description of each one is below. For more information refer to the online documentation. Tzero® Sample Encapsulating Press The TA Instruments Tzero sample encapsulating press is used to prepare encapsulated samples for DSC experiments.

  • Page 26: Installing The Discovery Dsc™ System

    • Installing a cooler option. It is recommended that you have your DSC installed by a TA Instruments Service Representative; call for an installation appointment when you receive your instrument. CAUTION: To avoid mistakes, read this entire chapter before you begin installation.

  • Page 27: Inspecting The System

    • If the instrument is damaged, notify the carrier and TA Instruments immediately. • If the instrument is intact but parts are missing, contact TA Instruments.
  • Page 28 CAUTION: Whenever plugging or unplugging power cords, handle them by the plugs, not by the cords. MISE EN GARDE: Chaque fois que vous branchez ou débranchez les cordons d'alimentation, tenez-les par les fiches et non par les cordons. WARNING: Protect power and communications cable paths. Do not create tripping hazards by laying the cables across access ways.
  • Page 29 USB 2.0 port Provides communications for external accessories. Micro USB 2.0 port Provides communications for external accessories. SD memory card slot For TA Instruments Service use only. CAN Communications Port Provides communications with external accessories. RS-232 Port Provides communications with external accessories.

  • Page 30: Setting Up System Communication

    Setting Up System Communication The instrument and controller must connect to an Ethernet router/switch for operation. The router can also be connected to a LAN to provide network storage and access, if desired. Refer to TRIOS Software Installation Instructions for more details. Connecting Lines to the Gas Delivery Module It is important to accurately control the atmosphere of the Discovery DSC cell during the experiment.

  • Page 31: Cooling Gas Line

    CAUTION: Corrosive gases cannot be used with this instrument. MISE EN GARDE: Des gaz corrosifs peuvent être utilisés avec cet instrument. WARNING: Use of flammable or explosive gas as a purge gas is dangerous and is not recom- mended for this instrument. AVERTISSEMENT: L'utilisation d'un gaz inflammable ou explosif comme gaz de drainage est dangereuse et n'est pas recommandée pour cet instrument.

  • Page 32: Connecting The Power Cable

    Connecting the Power Cable NOTE: A <HAR>-marked (harmonized) power cable meeting the standards of the country of installation is required for the European Economic Area. Install the power cable as follows: Make sure the power switch is in the Off (0) position, as shown in Figure Plug the power cable into the power entry module (shown below).

  • Page 33: Shutting Down The Discovery Dsc System

    Shutting Down the Discovery DSC System Before you decide to power down your system, consider the following: • All of the components of your thermal analysis system are designed to be powered on for long periods. • The electronics of the DSC perform more reliably if power fluctuations caused by turning units on and off are minimized.

  • Page 34: Installing The Dsc Cooling Accessories

    Installing the DSC Cooling Accessories The DSC operates in conjunction with one of several cooling accessories. Your choice of cooling accesso- ries depends on the temperature range required for your experiments. This section provides the information needed to install the FACS and Quench Coolers. For proper operation, the correct cooler type must be selected through the instrument control software.
  • Page 35 Place the FACS over the cell, aligning the orientation hole in the FACS with the pin on the instrument cell plate. Figure 12 Placing the FACS over the cell. Obtain a long 5/32-inch hexagonal (Allen) wrench from the accessory kit. Insert the tip of the wrench into any one of the three captive screws in the FACS plate and begin to tighten (3 to 4 turns).

  • Page 36: Installing The Refrigerated Cooling System (Rcs)

    Replace the top cover of the instrument and snap it into place. Figure 14 FACS fully installed. Select the correct cooler type on the Discovery DSC Cooler setting within the TRIOS software Options window. 10 You are now ready to use the FACS. This cooler requires a pressurized air source connected to the Cooling Gas fitting.
  • Page 37 Connect the two conductor cables exiting the rear of the cooling head base to the heater jacket harness. Figure 16 Unscrew the 2 screws holding the DSC cooler plug in place, and then remove the plug from the cover. Figure 17 Remove cooler plug. Discovery DSC™...
  • Page 38 Snap the DSC instrument cover back into place by inserting the tabs on the right side of the cover and then snapping the left side into position. Figure 18 Cover installed. Discovery DSC™ Getting Started Guide Page 37...

  • Page 39: Installing The Quench Coolers

    Installing the Quench Coolers Installing a Quench Cooler is slightly different depending on whether you are using the “stand-alone” vari- ety or the type to be used with the FACS. See the instructions below that apply to the desired type of Quench Cooler.

  • Page 40: Installing The Liquid Nitrogen Pump (Ln Pump)

    Place the thermal enclosure over the cell and align the notch in the plate with the alignment pin. Obtain a long 5/32-inch hexagonal (Allen) wrench from the accessory kit. Insert the tip of the wrench into any one of the three captive screws in the thermal enclosure plate and begin to tighten (3 to 4 turns at a time).

  • Page 41: Installing The Transfer Line

    Installation of the LN Pump involves: “Installing the Transfer Line” on page 40 “Installing the LN Pump to the Tank” on page 42 “Installing the LN Pump on the Discovery DSC” on page 43 Installing the Transfer Line Before the LN Pump can be installed on the Discovery DSC, the transfer line must first be attached to the LN Pump.
  • Page 42 Remove the insulation to expose the two fittings that will be attached to the feed hose. Using a 9/16-inch wrench, remove the liquid line connection cap. Then, using a 11/16-inch wrench, remove the return line connection cap. Liquid line connection Return line connection Figure 22 Connection caps.

  • Page 43: Installing The Ln Pump To The Tank

    Connect the transfer line to the LN Pump: Using a 9/16-inch wrench, attach the smaller liquid supply line to the smaller fitting. b Using an 11/16-inch wrench, attach the larger return line to the remaining fitting as shown in the figure below.

  • Page 44: Installing The Ln Pump On The Discovery Dsc

    MISE EN GARDE: Un mauvais alignement de la pompe sur le réservoir peut endommager le bouchon d'étanchéité sous vide. Pour éviter le risque de gel du capuchon d'étanchéité à vide, la fig- ure 26 montre l'orientation de la pompe vers le réservoir. Supply line Return line Relief valves: DO NOT ALIGN...
  • Page 45 Verify that the DSC cell surface (indicated in the figure below) on the top of the silver block is not damaged or compromised. If any irregularities such as dents, buildup, contaminants, or oxidation are observed in the silver, contact your local TA Instruments Service Representative for details on re-dressing the cell.
  • Page 46 CAUTION: Take extreme care not to damage the silver block shown in Figure 28. The silver surfaces on the cell are soft and, if damaged, must be replaced by a TA Instruments Service Representative. MISE EN GARDE: Soyez extrêmement prudent pour ne pas endommager le bloc en argent illustré...
  • Page 47 Insert the tip of the wrench into any one of the three captive screws in the LN Pump plate while holding onto the cooling head. You may need to push down while you tighten the screw 3 to 4 turns. DO NOT fully tighten yet.
  • Page 48 11 Once the cooling head is secured to the cell and the heater cable is properly installed, replace the top cover on the instrument. Connect the CAN communication cable to the DSC and the LN Pump connectors labeled “CAN.” 12 Select the correct cooler type on the Discovery DSC > Cooler setting within the TRIOS Software Options window.
  • Page 49 b Discovery DSC gas ports: GAS 1 port COOLING GAS port GAS 2 port Figure 35 Gas ports on back of Discovery DSC. Ensure that the pressure of your cooling gas is regulated to 140 kPa gauge (20 psig). Dry nitrogen should be used.

  • Page 50: Installation Of Additional Items

    Installing the Lid (DSC2500 only) The Discovery DSC2500 is shipped with two lids: a coated lid for operation up to 400°C, and a silver lid for operation up to 725°C. After unpacking the instrument and installing the instrument completely (see instructions in this chapter), you are ready to install a lid and run samples.
  • Page 51 Obtain the lid you wish to install and locate the notch on the top side of the lid. See the figure below. Lid notch Top of lid Figure 37 Top side of lid and lid notch. Gently grasp the sides of the AutoLid cover and slowly lift it to expose more of the lid pin. Lid cover being raised Lid support pin Figure 38 Lifting the insulated cover to expose the lid support pin.

  • Page 52: Use, Maintenance, & Diagnostics

    Chapter 3: Use, Maintenance, & Diagnostics Using the Discovery DSC™ All of your DSC experiments will have the following general outline. In some cases, not all of these steps will be performed. The majority of these steps are performed using the instrument control software. The instructions needed to perform these actions can be found in the online help in the instrument control software;...

  • Page 53: Calibrating The Discovery Dsc

    Calibration consists of several different types of procedures that are described briefly below. For more details on performing each type of calibration, refer to the instructions in online help. T1 Baseline Calibration (Discovery DSC2500, DSC250, DSC25) The baseline slope and offset calibration involves heating an empty cell through the entire temperature range expected in subsequent experiments.

  • Page 54: Enthalpy (Cell) Constant Calibration

    If multipoint temperature calibration is used, it is recommended that you choose standards that will bracket the desired measurement temperature range. This will ensure optimal calibration and performance. Heat Capacity Calibration (Discovery DSC2500 only) Heat capacity can be obtained in a single experiment with the Discovery DSC™. Heat capacity calibration is required to optimize the accuracy of the sample’s heat capacity.

  • Page 55: Autosampler Calibration

    Load the sample pan (and a similarly prepared empty reference pan) into the cell or onto the Autosampler tray. Enter experiment and procedure information through the TA Instruments TRIOS Software; this includes both sample and instrument information. Start the experiment.

  • Page 56: Starting An Experiment

    The primary maintenance procedures described in this section are the customer’s responsibility. Any fur- ther maintenance should be performed by a representative of TA Instruments or other qualified service per- sonnel. Consult the online help installed with the instrument control software for further information.

  • Page 57: Replacing Fuses

    The Discovery DSC™ contains internal fuses that are not user serviceable. If any of the internal fuses blows, a hazard may exist. Call your TA Instruments service representative. The only customer-replaceable fuses are the fuses located in the fuse holder located on the back panel of the instrument.

  • Page 58: Replacement Parts

    251470.010 Ethernet cable (10 foot, shielded) 253827.000 Power cord, 120 V North America 920223.902 Event cable *Contact your local TA Instruments representative for information on non-US style power cords. Table 6: Lids and Accessories Part Number Description 271580.001 Curved tweezers 972628.001...
  • Page 59 Table 8: Tzero Sample Encapsulation Press Part Number Description 901600.901 Tzero sample press kit (includes the press, the .901, .903, and .904 die sets given below, and 1 box each of Tzero aluminum pans (PN 901683.901) and Tzero aluminum lids (PN 901671.901) 901608.901 Die set for standard series pans (green)
  • Page 60 Table 10: Standard Series Pans and Lids Part Number Description 900578.901 Platinum pans (pkg of 10) 900786.901 Aluminum pans (pkg of 200) 900779.901 Aluminum lids (pkg of 200) 900793.901 Aluminum pans, hermetic (pkg of 200) 900794.901 Aluminum pans, hermetic (pkg of 200) 900860.901 Aluminum hermetic lids with pinhole (pkg of 50) 900796.901...
  • Page 61 Table 11: Calibration/Reference Materials Part Number Description 915060.901 DSC / DTA temperature calibration kit 915061.901 Replacement certified indium reference material for above kit 900902.901 Indium calibration material 900910.901 Tin calibration material 900907.901 Zinc calibration material 970345.901 Tzero sapphire calibration kit 970370.901 ®...

This manual is also suitable for:

Discovery dsc250Discovery dsc25

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