Related Manuals for TA Instruments DSC Q Series
Summary of Contents for TA Instruments DSC Q Series
- Page 1 Differential Scanning Calorimeter Q Series Getting Started Guide Revision N Issued January 2007...
- Page 2 ©2001–2007 by TA Instruments—Waters LLC 109 Lukens Drive New Castle, DE 19720 Notices The material contained in this manual, and in the online help for the software used to support this instrument, is believed adequate for the intended use of the instrument. If the instrument or procedures are used for purposes other than those specified herein, confirmation of their suitability must be obtained from TA Instruments. Otherwise, TA Instruments does not guarantee any results and assumes no obligation or liability. TA Instruments also reserves the right to revise this document and to make changes without notice. TA Instruments may have patents, patent applications, trademarks, copyrights, or other intellectual property covering subject matter in this document. Except as expressly provided in written license agreement from TA Instrument, the furnishing of this document does not give you any license to these patents, trademarks, copyrights, or other intellectual property. TA Instruments Operating Software, as well as Module, Data Analysis, and Utility Software and their associated manuals and online help, are proprietary and copyrighted by TA Instruments. Purchasers are granted a license to use these software programs on the module and controller with which they were purchased. These programs may not be duplicated by the purchaser without the prior written consent of TA Instruments. Each licensed program shall remain the exclusive property of TA Instruments, and no rights or licenses are granted to the purchaser other than as specified above. DSC Q Series Getting Started Guide...
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Page 3: Important: Ta Instruments Manual Supplement
Important: TA Instruments Manual Supplement Please click on the links below to access important information supplemental to this Getting Started Guide: • TA Instruments Trademarks • TA Instruments Patents • Other Trademarks • TA Instruments End‐User License Agreement • TA Instruments Offices 3 DSC Q Series Getting Started Guide... -
Page 4: Table Of Contents
Display Touch Screen Options ......................... 21 The DSC Q1000/Q100 Touch Screens ......................22 Primary Function Keys ..........................22 DSC Control Menu Keys ........................... 23 Display Menu Keys ............................ 24 DSC Auto Q20/Q20/Q10 Keypad ........................25 Options and Accessories ..........................26 Tzero Sample Encapsulating Press ......................26 DSC Autosampler ............................26 Photocalorimeter Accessory (PCA) ......................26 DSC Pressure Cell ............................27 Instrument Specifications ..........................28 DSC Instrument Characteristics ......................28 DSC Q Series Getting Started Guide... - Page 5 Heat Capacity (Q2000/Q1000) Calibration ..................... 50 Heat Capacity (MDSC®) Calibration ...................... 50 Pressure Calibration ..........................51 Autosampler Calibration .......................... 51 Q2000/Q200/Auto Q20 Autosampler Calibration ................51 Q1000/Q100 Autosampler Calibration .................... 53 Running a DSC Experiment ..........................54 Experimental Procedure ........................... 54 Loading the Sample ........................... 55 Starting an Experiment ..........................55 Stopping an Experiment ........................... 56 Maintaining the Instrument ..........................57 5 DSC Q Series Getting Started Guide...
- Page 6 Burning Off Contamination in a DSC Cell with an RCS or LNCS ..........59 Removing a DSC Q2000/Q1000 Cell ....................... 60 Installing a Cell ............................60 Replacing Fuses ..............................61 Replacing the DSC Fuses ........................... 61 Replacement Parts ............................. 62 Fuses, Cords, and Cables ........................62 DSC Cells, Lids, and Accessories ...................... 62 Autosampler Accessories ........................63 Tzero Sample Encapsulation Press ....................63 DSC Sample Pans, Lids, and Accessories ..................64 Calibration/Reference Materials ....................... 65 Index ................................... 67 DSC Q Series Getting Started Guide...
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Page 7: Notes, Cautions, And Warnings
A CAUTION emphasizes a procedure that may damage equipment or cause loss of data if not followed correctly. A WARNING indicates a procedure that may be hazardous to the operator or to the environment if not followed correctly. 7 DSC Q Series Getting Started Guide... -
Page 8: Regulatory Compliance
For Canada: CAN/CSA‐22.2 No. 1010.1‐92 Safety requirements for electrical equipment for measurement, control, and laboratory use, Part 1: General Requirements + Amendments. CAN/CSA‐22.2 No. 1010.2.010‐94 Particular requirements for laboratory equipment for the heating of materials + Amendments. For the European Economic Area: (In accordance with Council Directive 73/23/EEC of 19 February 1973 on the harmonization of the laws of Member States relating to electrical equipment designed for use within certain voltage limits.) EN61010‐1: 1993 Safety requirements for electrical equipment for measurement, control, and laboratory use, Part 1: General Requirements + Amendments. EN61010‐2‐010: 1994 Particular requirements for laboratory equipment for the heating of materials + Amend‐ ments. For the United States: UL61010A‐1 Electrical Equipment for Laboratory Use; Part 1: General Requirements. IEC 1010‐2‐010: 1992 Particular requirements for laboratory equipment for the heating of materials + Amend‐ ments. Electromagnetic Compatibility Standards For Australia and New Zealand: AS/NZS 2064: 1997 Limits and methods of measurement of electronic disturbance characteristics of industrial, scientific and medical (ISM) radiofrequency equipment. For Canada: ICES‐001 Issue 3 March 7, 1998 Interference‐Causing Equipment Standard: Industrial, Scientific, and Medical Radio Frequency Generators. For the European Economic Area: (In accordance with Council Directive 89/336/EEC of 3 May 1989 on the approximation of the laws of the Member States relating to electromagnetic compatibility.) EN61326‐1: 1997 Electrical equipment for measurement, control, and laboratory use‐EMC requirements‐Part 1: General Requirements + Amendments. Emissions: Meets Class A requirements (Table 3). Immunity: Meets performance criteria A for non‐continuous operation. For the United States: CFR Title 47 Telecommunication Chapter I Federal Communications Commission, Part 15 Radio frequency devices (FCC regulation pertaining to radiofrequency emissions). DSC Q Series Getting Started Guide... -
Page 9: Safety
You must unplug the instrument before doing any maintenance or repair work; voltages as high as 120/240 Vac are present in this system. WARNING: High voltages are present in this instrument. Maintenance and repair of internal parts must be performed only by TA Instruments or other qualified service personnel. 9 DSC Q Series Getting Started Guide... -
Page 10: Handling Liquid Nitrogen
Do not vent the Liquid Nitrogen Cooling System (LNCS) container in confined spaces. Do not enter confined spaces where high concentrations of nitrogen gas may be present unless the area is well ventilated. The warning above applies to the use of liquid nitrogen. Oxygen depletion sensors are sometimes utilized where liquid nitrogen is in use. DSC Q Series Getting Started Guide... -
Page 11: Thermal Safety
Thermal Safety 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. Lifting the Instrument The DSC is a fairly heavy instrument. In order to avoid injury, particularly to the back, please follow this advice: WARNING: Use two people to lift and/or carry the instrument. The instrument is too heavy for one person to handle safely. 11 DSC Q Series Getting Started Guide... - Page 12 DSC Q Series Getting Started Guide...
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Page 13: Chapter 1: Introducing The Dsc
Runs data analysis programs. NOTE: For technical reference information, theory of operation, and other information associ- ated with the DSC and not found in this manual, see the online help associated with the instrument control software. DSC Q Series Getting Started Guide... -
Page 14: Dsc System Components
Ohm's Law. This simple relationship, however, does not take into account extraneous heat flow within the sensor or between the sensor and sample pan. The TA Instruments Q Series DSC's are specifically designed to account for those latter heat flows. -
Page 15: Cooling Accessories
This term has its largest impact during enthalpic events (e.g., melting). This equation can be further modified to account for pan heat flow effects. TA Instruments supplies the following Q Series DSC's. • The Q20, Q10, and Auto Q20 instruments provide conventional (single-term) heat flow (commonly designated as "T1 heat flow") only. -
Page 16: Refrigerated Cooling System (Rcs)
The Refrigerated Cooling Systems (RCS) are used to perform DSC cooling experiments. There are two different models offered by TA Instruments—the RCS 90 and the RCS 40. Both models have a cooling head, which is made up of an internal heat exchanger, anti-condensate heaters, and various other components. The cooling head fits over the DSC cell. -
Page 17: Quench Cooler
The LNCS (Liquid Nitrogen Cooling System) is a universal cooling accessory for use with TA Instruments Analyzers. It can be used with all DSC Q Series models. The Liquid Nitrogen Cooling System (LNCS) allows auto- matic and continuous temperature control within the range of –180°C to 550°C. -
Page 18: The Dsc Q2000/Q200 Touch Screen
Items can be selected from the icons or from the drop-down menu. Select Apply to initiate the com- mand. See the next page for more details on this screen. (table continued) DSC Q Series Getting Started Guide... -
Page 19: Control Menu
Autosampler to "forget" the current lid and sample pan locations. UNLOAD Unloads the pan from the cell to the Autosampler tray or waste bin. LOAD Loads the selected pan from the Autosampler tray to the cell. (table continued) DSC Q Series Getting Started Guide... - Page 20 Toggles the RCS (Refrigerated Cooling System) between on and off, depending on the state of the RCS when you press the key. RESET SAVED PARAMETERS Resets the saved instrument parameters and resets the instru- ment. SHUTDOWN Shuts down and resets the instrument. DSC Q Series Getting Started Guide...
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Page 21: Display Touch Screen Options
Displays a time-based plot of data as it is received from the instru- ment during experiments. SCREEN SAVER Allows you to choose a screen saver for the touch screen. HOME Returns to the opening window. DSC Q Series Getting Started Guide... -
Page 22: The Dsc Q1000/Q100 Touch Screens
Displays the Control Menu touch screen keys. These are used to control certain instrument actions. Accesses the Display Menu screen, which is used to select the desired display option. DSC Q Series Getting Started Guide... -
Page 23: Dsc Control Menu Keys
Toggles between opening and closing the AutoLid on the cell. Takes you to the Autosampler touch screen display where you can calibrate the Autosampler and perform related functions. See the online help for information. DSC Q Series Getting Started Guide... -
Page 24: Display Menu Keys
Ensures proper shutdown of the instrument before turning off the power. Beeps the controller that is connected to the instrument. Returns to the opening window. DSC Q Series Getting Started Guide... -
Page 25: Dsc Auto Q20/Q20/Q10 Keypad
This is the same function as Stop on the instrument control software. Open/ (Available on Auto Q20 Only.) Toggles between opening and closing the Close DSC Auto Q20 Autolid. DSC Q Series Getting Started Guide... -
Page 26: Options And Accessories
Options and Accessories Several additional pieces of equipment are available from TA Instruments to be used with the DSC. A brief description of each one follows. For more information refer to the online documentation. Tzero Sample Encapsulating Press The TA Instruments Q Series Tzero Sample Encapsulating Press is used to prepare encapsulated samples for DSC experiments. -
Page 27: Dsc Pressure Cell
The cell has a pressure transducer which continuously measures actual sample pressure and stores it in the data file. This cell is optional for the Q2000 and Q1000. It comes standard on the Q20P and Q10P. DSC Q Series Getting Started Guide... -
Page 28: Instrument Specifications
RCS 40 -40 to 400 °C with LNCS -180 to 550 °C * You must use an inert atmosphere above 600 ** Helium purge gas must be used for temperatures below –100 °C (table continued) DSC Q Series Getting Started Guide... - Page 29 10 mm in hermetic pans Sample pans Various open or hermetically sealed (standard and Tzero series) Purge gases Recommended: air, argon, helium, nitrogen, or oxygen Typical purge flow rate 50 mL/min Cell volume 3.4 mL DSC Q Series Getting Started Guide...
- Page 30 DSC Q Series Getting Started Guide...
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Page 31: Chapter 2: Installing The Dsc
• Installing a transformer, if needed, for 230 Vac power 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 32: Choosing A Location
It is important to be certain that the instrument ground is adequately connected to the facilities ground for safe operation. Run the "Cell/Cooler Conditioning" test template to dry out the cell: 1 External Event Off 2 Equilibrate at 75°C 3 Isothermal for 120.00 min. DSC Q Series Getting Started Guide... -
Page 33: Connecting Cables And Lines
RCS and Differential Photocalorimeter (DPC) control. 24 Vdc output May be used for certain cooling accessories. Base Purge Used as an inlet port for nitrogen purge with the LNCS, QCA, and RCS cooling accessories. (table continued) DSC Q Series Getting Started Guide... - Page 34 Provides air for the Finned Air Cooling System (FACS) and nitrogen for the Refrigerated Cooling System (RCS). Base Purge Cooling Gas Gas 1 Gas 2 Four Ports on the Right Rear of the DSC DSC Q Series Getting Started Guide...
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Page 35: Ethernet Switch Setup
Computer yellow light will appear at the port. Ethernet Port Follow the directions in the next section to connect the controller to a LAN for networking capabilities. DSC Q Series Getting Started Guide... - Page 36 Check the Ethernet port on the rear of the computer. If communication between the computer and the LAN has been properly established, a solid green light and flashing yellow light will appear at the port. Ethernet Connection DSC Q Series Getting Started Guide...
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Page 37: Purge Lines
WARNING: Use of an explosive gas as a purge gas is dangerous and is not recommended for this instrument. For a list of the purge gases that can be used with the DSC instrument, see Chapter 1. DSC Q Series Getting Started Guide... -
Page 38: Cooling Gas Line
Connect the gas line to the Base Purge port using 1/8-inch O.D. tubing. Teflon® TFE tubing is recommended. An orifice in the instrument will automatically regulate the flow rate (300 to 350 mL/min) for proper operation. DSC Q Series Getting Started Guide... -
Page 39: Voltage Configuration Unit
10 amp fuses with 6.3 amp fuses, which are supplied in the kit. Dis- card the 10 amp fuses. See the figure Captive Fasteners to the right. Voltage Configuration Unit DSC Q Series Getting Started Guide... -
Page 40: Power Switch
Set the instrument power switch to the ON (1) position. After the proper power up sequence, the TA Instruments logo will be displayed on the touch screen or the green light on the keypad will be lit, this indicates that the instrument is ready for use. -
Page 41: Shutting Down The Dsc
To power down your instrument set the power switch to the OFF (0) position. DSC Q Series Getting Started Guide... -
Page 42: Installing The Dsc Cooling Accessories
If you do not have an Autosampler, you will have to remove additional screws to release the cover. Then pull the cover towards you to remove it fully. DSC Q Series Getting Started Guide... -
Page 43: Installing The Quench Coolers
Slide the cooler into place into the top of the Finned Air Cooling System (FACS) using gloves to handle it, if you have already poured liquid nitrogen into it as shown in the figure here. DSC Q Series Getting Started Guide... -
Page 44: Quench Cooler
You will need to exert downward pressure on the wrench while you tighten the screw a few turns. DO NOT fully tighten yet. Alignment Pin DSC Q Series Getting Started Guide... - Page 45 "Stand-Alone" Quench Cooler and Cooling Head NOTE: The Quench Cooler may only be used to obtain Heat Flow T1. DSC Q Series Getting Started Guide...
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Page 46: Installation Of Additional Items
Installation of Additional Items Several additional items can be found in the accessory box that is shipped with your instrument. While your TA Instruments Representative may install many of these for you, it is important to know how to install them yourself. -
Page 47: Chapter 3: Use, Maintenance, & Diagnostics
• Connected all gas lines • Powered up the unit • Connected any desired accessories • Connected the instrument with the controller • Become familiar with controller operations • Calibrated the DSC, if necessary. DSC Q Series Getting Started Guide... -
Page 48: Calibrating The Dsc
✔ with pressure cell * Tzero™ describes proprietary technology invented by Robert Danley of TA Instruments—Waters LLC and patented by TA Instruments—Waters LLC (U.S. Patent No. 6,431,747). ** Heat Capacity calibration is NOT performed in cal mode and is not required except when making absolute measurements of heat capacity. -
Page 49: Tzero Tm
This calibration is used in the DSC Auto Q20, Q20, and Q10 and when the selected heat flow is T1 for the other DSC models. DSC Q Series Getting Started Guide... -
Page 50: Enthalpy (Cell) Constant Calibration
Reversing Heat Capacity to the default values of 1.0. Except for heating rate, the calibration experiment should be run under similar conditions (pan type, modulation amplitude, and period) to those that will be used DSC Q Series Getting Started Guide... -
Page 51: Pressure Calibration
The screen shown in the figure to the right will be displayed. b. Press the Autosampler button. Touch the Calibration tab, if it is not already selected. The screen shown on the next page is displayed. DSC Q Series Getting Started Guide... - Page 52 See the online help for detailed information. Make sure you press the Save button when you have finished the desired calibration function. After calibration is complete, you can perform a Cycle Test to test the calibrated positions. DSC Q Series Getting Started Guide...
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Page 53: Q1000/Q100 Autosampler Calibration
See the online help for detailed information. Make sure you save the calibrations when you have finished the desired calibration function. After calibration is complete, you can perform a Cycle Test to test the calibrated positions. DSC Q Series Getting Started Guide... -
Page 54: Running A Dsc Experiment
Loading the sample pan (and a similarly prepared empty reference pan) into the cell or onto the Autosampler tray. • Entering experiment and procedure information through the TA controller, this includes both sample and instrument information. • Starting the experiment. DSC Q Series Getting Started Guide... -
Page 55: Loading The Sample
Start the experiment by by selecting Start on the instrument control software, touching the START key on the instrument touch screen, or by pressing the Start key on the keypad (Auto Q20/Q20/Q10). When you start the instrument, the system automatically runs the experiment to completion. DSC Q Series Getting Started Guide... -
Page 56: Stopping An Experiment
Another function that stops the experiment is REJECT. However, the Reject function discards all of the data from the experiment; the Stop function saves any data collected up to the point at which the experiment was stopped. DSC Q Series Getting Started Guide... -
Page 57: Maintaining The Instrument
The primary maintenance procedures described in this section are the customer’s responsibility. Any further maintenance should be performed by a representative of TA Instruments or other qualified service personnel. Consult the online documentation installed with the instrument control software for further information. -
Page 58: Burning Off Contamination In A Dsc Cell With A Facs Installed
Then remove the residue from the cell using clean compressed air. • Run a baseline (empty cell). If there is an improvement relative to the baseline before “burn off” but the baseline is still unacceptable, repeat the procedure above. DSC Q Series Getting Started Guide... -
Page 59: Burning Off Contamination In A Dsc Cell With An Rcs Or Lncs
If the baseline problem remains, it is probably not due to contamination; the cell may need to be replaced (contact your TA Instruments service representative). • Once the baseline is acceptable, return to normal operation. DSC Q Series Getting Started Guide... -
Page 60: Removing A Dsc Q2000/Q1000 Cell
To install a cell on the Q2000/Q1000, slide the cell into place fully engaging the connectors. Thumbscrews Tighten the thumbscrews equally until they cannot be tightened further—do not force. Then reverse the directions given in the previous section to reinstall the cover. DSC Q Series Getting Started Guide... -
Page 61: Replacing Fuses
Replacing the DSC Fuses The 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 fuses that you can replace yourself are the fuses... -
Page 62: Replacement Parts
Replacement Parts Replacement parts for the DSC that are available from TA Instruments. See the tables below when ordering parts. Fuses, Cords, and Cables Part Number Description 205221.001 Fuse (6.3 amp, 250 V) 205221.002 Fuse (10 amp, 250 V) 205224.035 Fuse (0.75 amp, 250V Slo Blo) for 230V/50Hz RCS... -
Page 63: Autosampler Accessories
Tzero Aluminum pans (PN 901670.901) and Tzero Aluminum Lids (PN 901671.901) 901608.901 Replacement Die Set for Standard Series Pans 901608.903 Replacement Die Set for Tzero Series Aluminum Pans 901608.904 Replacement Die Set for Tzero Series Hermetic Pans and Tzero Series Hermetic Alodined Pans DSC Q Series Getting Started Guide... -
Page 64: Dsc Sample Pans, Lids, And Accessories
Graphite Lids (Pkg of 10) 900825.901 High Volume Pan Kit (Includes metal bell jar, & lid, dies set, pans, lids, seals) 900824.901 High Volume Pan Die Set 900825.902 High Volume Pans, Lids & Seals (100 of each) (continued) DSC Q Series Getting Started Guide... -
Page 65: Calibration/Reference Materials
900907.901 Zinc Calibration Material 970345.901 Tzero™ Sapphire Calibration Kit 970370.901 MDSC® Sapphire Calibration Kit 915079.901 Sapphire Specific Heat Material 899096.901 Anisic Acid (1 g) 899097.901 Biphenyl (1 g) 900319.901 DSC Oxidative Stability Calibration Kit DSC Q Series Getting Started Guide... - Page 66 DSC Q Series Getting Started Guide...
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Page 67: Index
Autosampler calibration AUTOSAMPLER key base purge line base purge port cable Ethernet cables connecting Calibrate calibration Autosampler heat capacity MDSC heat capacity pressure cell burning out cleaning installing removing DSC Q Series Getting Started Guide... - Page 68 Differential Scanning Calorimeter (DSC) additional accessories sample encapsulating press basic experimental steps calibrating description experiments removing a cell (DSC Q2000/Q1000) dimensions Display Display Menu Q1000/Q100 DISPLAY MENU key Display Options Q2000/Q200 DSC Q Series Getting Started Guide...
- Page 69 Event port exothermic reaction experiment procedure rejecting starting stopping experiments basic steps Finned Air Cooling System (FACS) installing quench cool accessory fuses replacing on DSC Gas 1 port DSC Q Series Getting Started Guide...
- Page 70 Finned Air Cooling System (FACS) Quench Cool Accessory for FACS Quench Cooler voltage configuration unit instrument additional accessories pressure cell sample encapsulating press Autosampler choosing a location components connecting to Ethernet switch cooling accessories DSC Q Series Getting Started Guide...
- Page 71 (DSC Q20/Q10) installing liquid nitrogen handling 17, 38 Liquid Nitrogen Cooling System (LNCS) 20, 23 LNCS LNCS (Liquid Nitrogen Cooling System) description Load loading samples location of instrument maintenance Mass Flow Controller (MFC) DSC Q Series Getting Started Guide...
- Page 72 Gas 1 Gas 2 power cable installing power entry module power switch pressure calibration Pressure DSC (PDSC) cell primary function keys Q1000/Q100 Q2000/Q200 purge gases flow rate recommended Quench Cool Accessory for FACS installing DSC Q Series Getting Started Guide...
- Page 73 Reset Autosampler Reset Saved Parameters robotic device running experiments Safety burns electrical safety thermal Safety Standards sample loading Sample Encapsulating Press sample pans sample size sample tray installing sample volume Screen saver key screws DSC Q Series Getting Started Guide...
- Page 74 Status key 18, 22 status line Stop STOP key Stop key stopping instrument stopping an experiment SWITCH GAS Switch Gas temperature range thermal safety touch screen cleaning primary function keys Q1000/Q100 Q2000/Q200 DSC Q Series Getting Started Guide...
- Page 75 ultraviolet light Unload Unload Reference unpacking visible light voltage configuration unit installing weight...
- Page 76 DSC Q Series Getting Started Guide...