593M 6755 Solution Calorimeter Operating Instruction Manual For models produced after November 2010
Table of Contents Preface Scope — 1 Chapter 5 Calculations Related Instructions — 1 Standardization — 22 Customer Service — 1 Calculating the Energy Change — 23 Explanation of Symbols — 2 Reading the Thermogram — 23 Safety Information — 3 Intended Usage — 3 General Specifications — 3 Environmental Conditions — 3 Provisions for Lifting and Carrying — 3 Cleaning & Maintenance — 3 Specifications — 3 Chapter 1 Installation Power Connection — 4 Motor Installation — 4 Thermistor Probe Installation — 4 Cha
6755 Preface PREFACE Scope This manual contains instructions for installing and operating the Parr 6755 Solution Calorimeter. For ease of use, the manual is divided into 14 chapters.
Preface Explanation of Symbols I On Position O Off Position ~ Alternating Current This CAUTION symbol may be present on the Product Instrumentation and literature. If present on the product, the user must consult the appropriate part of the accompanying product literature for more information. ATTENTION, Electrostatic Discharge (ESD) hazards. Observe precautions for handling electrostatic sensitive devices. Protective Earth (PE) terminal.
6755 Safety Information To avoid electrical shock, always: 1. Use a properly grounded electrical outlet of correct voltage and current handling capability. 2. Ensure that the equipment is connected to electrical service according to local national electrical codes. Failure to properly connect may create a fire or shock hazard. 3. For continued protection against possible hazard, replace fuses with same type and rating of fuse. 4. Disconnect from the power supply before maintenance or servicing.
1 Installation CHAPTER 1 Installation The 6755 Solution Calorimeter requires approximately 4 square feet of work space on a sturdy bench/table in a location free from room drafts or radiant heat sources, (preferably in an air conditioned room providing minimal temperature change), and an electrical outlet. Other necessary accessories include: • Chemical balance sensitive to 0.1 mg • Top loading balance capable of weighing up to 1.5 kg with a sensitivity of 0.
6755 Installation Figure 1 2X SA1332RP06 6-32 X 3/8 RHMS PHILLIPS 2X SA1140RP04 4-40 X 1/4 RHMS PHILLIPS 327C2 BACK PANEL (REF) SA1332RP06 6-32 X 3/8 RHMS PHILLIPS (SEE NOTE) 493E Plug with 3280HC Retainer installed to insulate from live circuits when no motor is attached. BACK VIEW 95F DATA LABEL NOTE: CONNECT UNTERMINATED 493E WITH 328HC BRACKET TO THE MOTOR OUTPUT RECEPTACLE SECURING IT USING THE SA1332RP06 FASTENER. 6772 Calorimetric Thermometer Back Panel www.parrinst.
2 Quick Start CHAPTER 2 Quick Start Before starting to use the calorimeter for the first time, it is recommended that the user perform a dry run with the calorimeter completely assembled, but with no liquid in the Dewar and no sample in the rotating cell. This will give the user an opportunity to become familiar with the individual parts of the calorimeter and the manner in which they must be handled. The calorimeter must be standardized prior to analyzing a sample. See Chapter 3: Operation for more detail.
6755 Notes www.parrinst.
3 Operation CHAPTER 3 Operation Menu System All configurations and operations are handled by a menu-driven system operated from the bright touch screen display. The settings and controls are organized into eight main sections as displayed on the MAIN MENU. 4. Data Displays. Most of these keys display values that have been calculated by the Calorimetric Thermometer and are informational only. Certain ones can be overridden by the user entering a desired value through a sub-menu.
6755 Operation Note: Changes to the program are made by use of the menu structure. Any of these items can be individually entered at any time to revise the operating program. Default Settings The 6772 Calorimetric Thermometer is preprogrammed with default settings for use with the 1341 Plain Jacket Calorimeter. On the operating controls page of the 6772 Thermometer is the Method of Operation key. This key toggles the thermometer between solution and combustion calorimetry.
3 Operation Sample Size The rotating sample cell will hold up to 20 ml of liquid sample or a solid sample weighing up to one gram. More than one gram of solid may be used in some cases, but smaller samples are preferred so that the heat capacity and ionic strength of the system will not change significantly when the reactants are mixed. The Dewar must be filled with not less than 90 ml and not more than 120 ml of liquid to properly cover the rotating cell.
6755 Emptying the Calorimeter Stop the calorimeter motor, raise the cover carefully and wipe any excess liquid from the parts that were immersed in the Dewar. Remove the thermistor probe from the cover and remove the sample dish from the end of the push rod; then remove the rod and release the glass cell from the drive shaft. Lift the Dewar out of the air can and empty it; then wash and dry all wetted parts carefully.
4 Menu Descriptions CHAPTER 4 Menu Descriptions Note: Keys which make global changes to the setup of the calorimeter contain a YES or NO response to make certain that the user wishes to proceed. This two step entry is intended to prevent inadvertent global program changes. Calorimeter Operation Menu The Calorimetric Thermometer will normally be operated from the Calorimeter Operation Menu, although tests can always be started from any menu screen.
6755 Temperature Plot Setup Menu Menu Descriptions Jacket Min Value: Press this key to access its numeric dialog box to set a minimum jacket value. Time Window: Sets the time scale for the Xaxis. Time Units: Toggles between minutes and seconds. Enable Bucket: Toggles ON/OFF. Bucket Autoscale: Toggles ON/OFF. Enable Jacket: Toggles ON/OFF. Jacket Autoscale: Toggles ON/OFF. Time Mode: Toggles between Autoscale, Window, and Range.
4 Menu Descriptions Operating Controls Menu LCD Backlight Intensity: This key accesses a submenu with a slide control which adjusts the brightness on the LCD display for optimum viewing. Print Error Messages: When turned ON, all error messages will be printed on the printer as well as displayed on the screen. When turned OFF, messages will only display on the screen. Language: Steps the Calorimetric Thermometer through the installed operating languages.
6755 Date & Time Settings Menu Descriptions User/Factory Settings Date: Displays current date and accesses the sub-menu on which the date is set (YY/MM/ DD) format. Reload Factory Default Settings: Used to erase all of the settings and restore the factory default settings. Time: Display current time and accesses the sub-menu on which time is set in (HH:MM) format.
4 Menu Descriptions Data Entry Controls Menu Next Auto Sample ID Number: Establishes the initial sample number for a series of tests and then shows the next sample ID which will be assigned. Used when the Automatic Sample ID is set to ON. Press this key to access a submenu for entering a numeric increment. Auto Sample ID Increment: Establishes the increment between sample numbers; used when the Automatic Sample ID is set to ON. Press this key to access a sub-menu for entering a numeric increment.
6755 Communication Controls Menu Accesses sub-menus which set the communications protocols for the printer and balances. Menu Descriptions Balance Port Communications Balance Type: Toggles through the available balance templates. Printer Type: Toggles between a Parr 1758 and a generic printer. When set for the 1758 Printer, all of the features of this printer, such as bold printing, will be activated. Balance Port: Accesses sub-menu, Balance Port Communications.
4 Menu Descriptions Balance Port Settings 18 » Number of Data Bits. Standard options for data bits. Toggles between 7 and 8. » Parity. Standard options for parity. Choose from None, Odd or Even. » Number of Stop Bits. Standard options for stop bits. Toggles between 1 and 2. » Handshaking. Standard options for handshaking. Choose from Xon / Xoff, RTS/ CTS and None. » Baud Rate. Standard options for baud rate. Choose from 19.2K , 9600, 4800, 2400, 1800, 1200, 600, 300, 150, 134.5, 110, and 75.
6755 File Management Menu Run Data File Manager: This key activates the File Manager. The File Manager is used to delete or rename test report files. It is also used to convert file types. Run Data File Manager Menu Descriptions » Select: This key is used to begin the file selection process. The up / down and page up / page down keys are used to scroll up and down the file list. Pressing the select key when a file is highlighted blue will highlight the file with a cyan color.
4 Menu Descriptions Diagnostics Menu Provides the user with the means to test many of the components and subsystems of the Calorimetric Thermometer. These capabilities should be used in conjunction with the Maintenance Instructions in order to obtain the maximum benefits from these capabilities. Data Logger Controls Data Logger: This key toggles the data logging function ON/OFF.
6755 Data Log Format: Toggles between Text Format and Data Format (csv). Data is either logged with the supporting tag information (text) or in a comma separated variable (csv) data format as selected by the user. The text setting is useful if the data log destination is a printer. The data (csv) format is especially useful if the data is ultimately transferred to another computer for post processing, graphing etc. The log file can be transferred to another computer via FTP or SD Card.
5 Calculations CHAPTER 5 Calculate the energy equivalent of the calorimeter and its contents by substituting in the equation: Calculations Standardization A sample of tris (hydroxymethyl) aminomethane, commonly called TRIS, is furnished with the 6755 Calorimeter to provide a reliable standardizing reagent.
6755 Calculations Calculating the Energy Change The energy change, Q, measured in this calorimeter is calculated by multiplying the net corrected temperature change, ∆Tc, by the energy equivalent, e, of the calorimeter and its contents. Q = (∆Tc)(e) If ∆Tc is measured in °C and e is expressed in calories per °C, Q will be reported in calories. (The energy equivalent, e, is determined by a standardization procedure).
5 Calculations Example - Exothermic Reaction Problem: Determine the change in enthalpy for solid sodium sulfate, Na2SO4, when dissolved in a 5 gram/liter aqueous solution of barium chloride, BaCl2 • 2H2O. Na2SO4 m = 0.1458 grams Ba solution = 100.00 grams ++ = = = = = -34.99 cal/g @ 24.885 °C Or, multiplying by 142.04 (the molecular weight of Na2SO4) Corrected temperature rise ∆TC T(0.63R) Enthalpy change 0.042 °C (from Figure 3) 24.885 °C = (-34.99) (142.04) = -4.970 Kcal/mole @ 24.
6755 Calculations Example - Endothermic Reaction Problem: Determine the heat of solution of solid potassium nitrate, KNO3, when dissolved in water. Enthalpy change = KNO3 m = 0.7180 gram = Distilled water = 100.00 grams = -34.99 cal/g @ 24.885 °C Corrected temperature rise ∆TC T(0.63R) = = Or, multiplying by the molecular weight of KNO3 -0.508 °C (from Figure 3) 25.400 °C = (85.94) (101.10) = 8.69 Kcal/mole @ 25.400 °C Energy equivalent e = 121.
6 Reports CHAPTER 6 Reports The 6772 Calorimetric Thermometer can transmit its stored test data in either of two ways. The Auto Report Destination key on the Reporting Controls Menu toggles the report destination between the display and an optional printer connected to the USB printer port of the Calorimetric Thermometer. Test results are stored as files using the sample ID number as the file name. A listing of the stored results is accessed by pressing the REPORT command key.
6755 Memory Management CHAPTER 7 Memory Management The 6772 Calorimetric Thermometer will hold data for 1000 tests in its memory. These tests may be pre weights, preliminary or final reports for either calibration or determination runs. Once the memory of the controller is filled, the controller will not start a new analysis until the user clears some of the memory. The FILE MANAGEMENT key on the main menu leads to the file management submenu. The RUN DATA FILE MANAGER key leads to a listing of the files.
8 Accessory Connections CHAPTER 8 Accessory Connections Communication Connection There is a USB connection on the rear of the 6772 to facilitate printer and balance connections. The 6772 will allow the user to specify the IP addresses of one or more Balance Interface devices on the network by selecting the Network Data Device menu in the Communications Controls menu. Balance Interface devices are polled from device 1 to 15 for sample and / or spike weights when the weight entry mode is set to Network.
6755 Bar Code Port The use of barcodes in the laboratory has become a highly accurate, rapid and inexpensive way to identify samples. When purchasing this feature, the user must supply Parr with the MAC address of the calorimeter (found in the Software & Hardware Info menu screen). This allows Parr to activate the feature key. In order to enable the calorimeter to use the bar code feature, the feature key needs to be entered into the instrument.
8 Accessory Connections The following screenshot illustrates the contents of the Calorimetric Thermometer data directory as presented by a web browser. You can drag and drop or copy and paste test data files (with the csv suffix) from the web browser window to any convenient folder or directory on the PC.
6755 Accessory Connections The Calorimetric Thermometer offers a web server service. Test reports can be viewed with a web browser using a URL of the following form. http://10.1.5.100 Where 10.1.5.100 is the IP address of the Calorimetric Thermometer. The following screenshot illustrates the Calorimetric Thermometer status page. www.parrinst.
8 Accessory Connections Clicking on the Config tab displays some of the configuration options available in the 6772. Changes made on this page will change the settings in the 6772.
6755 Accessory Connections Clicking on the Run Data tab displays a list of reports currently in the instrument memory. Clicking on any given report will provide a display similar to the following: www.parrinst.
8 Accessory Connections Clicking on System Info will bring up the Software and Hardware Info screen from the 6772.
6755 Accessory Connections Clicking on the LCD Snapshot Page will bring up an image of the current display on the 6772. Note that this is a picture only. To operate the 6772 from a PC a Remote Feature Key must be installed. Please contact Parr Instrument Company for more details. www.parrinst.
8 Accessory Connections Clicking on Documentation will provide links to the manual and other helpful documents. Note: a connection to the Internet is required to access the documentation.
6755 Remote Operation (Optional) The 6772 can be operated remotely via PC over a network with the purchase of the 1965E Remote Feature Key. Samba Server Feature (Optional) Samba was originally developed as an implementation of the SMB (Server Message Block) protocol. The most common use of SMB is in Mircosoft’s CIFS (Common Internet File System) implementation. As a result, Samba has become a de facto Microsoft network compatibility tool.
9 Maintenance CHAPTER 9 Maintenance Examine the rotating cell periodically for leaks by closing the cell and submerging the empty bell in a beaker of water for a period of time comparable to a complete run in the calorimeter. If water migrates into the sealing area between the PTFE dish and the glass bell, the seal is deteriorating and the 126C PTFE dish should be replaced.
6755 Troubleshooting 10 CHAPTER 10 Troubleshooting Error List The calorimeter will run a number of diagnostic checks upon itself and will advise the operator if it detects any error conditions. Most of these errors and reports will be self-explanatory. The following list contains errors that are not necessarily self-evident and suggestions for correcting the error condition. A Misfire Condition Has Been Detected. This error will be generated in the event the total temperature change fails to exceed 0.
11 Technical Service CHAPTER 11 Contact Us Technical Service Technical Service Department Should you need assistance in the operation or service of your instrument, please contact the Technical Service Department. 1-309-762-7716 • 1-800-872-7720 • Fax: 1-309-762-9453 E-mail: parr@parrinst.com • http://www.parrinst.com Any correspondence must include the following basic information: • The model and serial # of the instrument. • Date purchased.
6755 Parts List 12 CHAPTER 12 Parts Lists Parts for the 6755 Solution Calorimeter Part Number Description A338CEB Stirrer Drive Motor Assembly 115V A338CEE Stirrer Drive Motor Assembly 230V A120C Calorimeter Cover with Stirrer Hub & Bearing Assembly 122C Locating Ring (6755) 123C Dewar Flask 150 mL 126C Sample Dish, PTFE 128C Hollow Shaft A129C Push Rod Assembly A130C Sample Cell with Coupling, less 126C Dish 132C Bushing for 133C Stirrer Pulley 133C Stirrer Pulley 135C Drive Belt
13 Drawings CHAPTER 13 Drawings External Parts View of 6755 Solution Calorimeter 42 Parr Instrument Company
6755 Drawings 13 Internal Parts View of 6755 Solution Calorimeter www.parrinst.
A2140E IO BOARD 44 Parr Instrument Company A2154E CPU BOARD CONNECTS IN LOWER PORT OF J4 ON CPU A2166E IO TO CPU USB CABLE ASSY (RED WIRE ON CABLE CONNECTS TO PIN #1) PIN #1 PIN #1 A1822E POWER CABLE ASSY J10 J1 J9 J8 J4 J100 J19 J17 J6 J5 2147E LCD DISPLAY CONNECTS IN UPPER PORT OF J4 OF CPU A2167E USB PERIPHERAL CABLE ASSY A2163E LCD CABLE ASSY A1823E2 TOUCH SCREEN CABLE ASSY A1821E SPEAKER CABLE ASSEMBLY A2164E BACKLIGHT CONTROL CABLE ASSY BACK PANEL USB PORT J8 J2 J9 J6 J1
www.parrinst.com 190F (REF) 2X 340C STANDOFF, 6-32 THD X 3.
13 Drawings Internal Parts View of 6772 Calorimetric Thermometer 2X TN1332HL 6-32 HEX KEPS NUT (1262DD BRKT MTG) 1940E POWER SUPPLY 2X TA030MFP05 3mm X 5mm FHPMS A59A4 BINDING POST, BLACK A59A2 BINDING POST, RED Note: 1262DD Capacitor Bracket and 897E Capacitor not shown for clarity.
6755 13 Drawings Back Panel of 6772 Calorimetric Thermometer 2X SA1332RP06 6-32 X 3/8 RHMS PHILLIPS 2X SA1140RP04 4-40 X 1/4 RHMS PHILLIPS 327C2 BACK PANEL (REF) SA1332RP06 6-32 X 3/8 RHMS PHILLIPS (SEE NOTE) 493E Plug with 3280HC Retainer installed to insulate from live circuits when no motor is attached. BACK VIEW 95F DATA LABEL NOTE: CONNECT UNTERMINATED 493E WITH 328HC BRACKET TO THE MOTOR OUTPUT RECEPTACLE SECURING IT USING THE SA1332RP06 FASTENER. www.parrinst.
14 Default Settings CHAPTER 14 Default Settings The following are recommended operation settings for the 6755 Solution Calorimeter.
Revision 07/08/13
