Operating Instruction Manual 591M 6772 Calorimetric Thermometer Operating Instruction Manual For models produced after November 2010
6772 Calorimetric Thermometer Instruction Manual TABLE OF CONTENTS TABLE OF CONTENTS ....................................................................................................... 1-1 PREFACE ............................................................................................................................ 1-1 Scope................................................................................................................................ 1-1 Explanation of Symbols .....................
6772 Calorimetric Thermometer Instruction Manual Diagnostics Menu ........................................................................................................... 5-19 CALCULATIONS ................................................................................................................. 6-1 Corrections ....................................................................................................................... 6-1 Manual vs. Fixed Corrections .....................................
6772 Calorimetric Thermometer Instruction Manual PREFACE Scope This manual contains instructions for installing and operating the Parr 6772 Calorimetric Thermometer with the 1341 Plain Jacket Calorimeter. For ease of use, the manual is divided into 13 chapters. Installation Quick Start Operation Menu Descriptions Calculations Reports Memory Management Maintenance Troubleshooting Technical Service Parts Lists Drawings Tables Subsections of these chapters are identified in the Table of Contents.
6772 Calorimetric Thermometer Instruction Manual Note: The unit of heat used in this manual is the International Table (IT) calorie, which is equal to 4.1868 absolute joules. Specific instructions for use of the 6772 with the Solution Calorimeter, Model 6755 are included in manual number 593M. Instructions for using the 6772 Calorimetric Thermometer with the 6725 Semimicro Calorimeter are included in manual number 592M.
772 Calorimetric Thermometer Instruction Manual Intended Usage If the instrument is used in a manner not specified by Parr Instrument Company, the protection provided by the equipment may be impaired. General Specifications Electrical Ratings 115VAC, 1.0 Amp, 50/60 Hz 230VAC, 1.
6772 Calorimetric Thermometer Instruction Manual INSTALLATION Power Connection Plug the power line into any grounded outlet providing proper voltage that matches the specification on the nameplate of the Calorimetric Thermometer. The thermometer will draw approximately 100 watts of power. Grounding is very important not only as a safety measure, but also to ensure satisfactory controller performance.
6772 Calorimetric Thermometer Instruction Manual Thermistor Probe Installation Connections for two thermistor probes are located on the back of the 6772 Calorimetric Thermometer. If only one probe is to be used, connect it to the “bucket” connection. The 6772 Calorimetric Thermometer includes an ignition unit for automatically firing the bomb in the 1341 calorimeter.
6772 Calorimetric Thermometer Instruction Manual Communication Connection There is a USB connection on the rear of the 6772 to facilitate printer and balance connections. The 6772 will also 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.
6772 Calorimetric Thermometer Instruction Manual The format of an unknown balance can be determined by logging the balance output to the printer attached to the Calorimetric Thermometer. Those protocols which send a command string to the balance will do so while logging is active. In order for the logging to produce meaningful results, the cable connecting the balance to the balance input port of the Calorimetric Thermometer must be correctly wired or configured.
6772 Calorimetric Thermometer Instruction Manual 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. Select the “Program Information and Control” key from the Main Menu. Next, select “Feature Key” and enter the feature key purchased from Parr Instrument Company into the instrument by using the touchpad.
6772 Calorimetric Thermometer Instruction Manual 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.
6772 Calorimetric Thermometer Instruction Manual 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://192.168.0.125 Where 192.168.0.125 is the IP address of the Calorimetric Thermometer. The following screenshot illustrates the Calorimetric Thermometer status page.
6772 Calorimetric Thermometer Instruction Manual 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.
6772 Calorimetric Thermometer Instruction Manual Clicking on the Run Data tab displays a list of reports currently in the instrument memory.
6772 Calorimetric Thermometer Instruction Manual Clicking on System Info will bring up the Software and Hardware Info screen from the 6772.
6772 Calorimetric Thermometer Instruction Manual 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.
6772 Calorimetric Thermometer Instruction Manual 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.
6772 Calorimetric Thermometer Instruction Manual QUICK START The basic operating instructions for the 1341 Calorimeter are found in Operating Instructions Manual No. 204M. Detailed instructions for preparing the sample and charging the 1108 Oxygen Bomb are given in the operating instructions, manual number 205M. Follow these instructions carefully, giving particular attention to the precautions to be observed in charging and handling the bomb.
6772 Calorimetric Thermometer Instruction Manual ID number, sample ID number, sample weight and spike weight in accordance with the instructions set into the operating controls page. 8. The thermometer will now take over and conduct the test. During the time it is establishing the initial equilibrium, it will display PREPERIOD on the status bar. Just before it fires the bomb, it will sound a series of short beeps to warn the user to move away from the calorimeter.
6772 Calorimetric Thermometer Instruction Manual 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 ten main sections as displayed on the MAIN MENU. Note: Keys with a “double box” in the upper left hand corner lead to sub-menus. Menu Keys The controls that change the data field information in the menus will be one of the following: 1. Toggles.
6772 Calorimetric Thermometer Instruction Manual 4. Report. This key is used to access the test results stored in the Calorimetric Thermometer, to enter thermochemical corrections, and to initiate a report on the display, printer or attached computer. 5. Help. This key is used to access help screens related to the menu currently displayed on the touch screen. 6. This key appears in the Escape key location when the main menu is displayed.
6772 Calorimetric Thermometer Instruction Manual corrections to the calorimeter temperature rise in order to correct for all systemic heat leak effects. In either case the operator must determine the appropriate temperature source for the jacket.
6772 Calorimetric Thermometer Instruction Manual Fill the calorimeter bucket by first taring the dry bucket on a solution or trip balance; then add 2000 (± 0.5) grams of water. Distilled water is preferred, but demineralized or tap water containing less than 250 ppm of dissolved solids is satisfactory. The bucket water temperature should be approximately 1 - 2 °C below the room temperature. It is not necessary to use exactly 2000 grams, but the amount selected must be duplicated within ± 0.
6772 Calorimetric Thermometer Instruction Manual and combustion capsule) with a jet of distilled water and collect the washings in a beaker. Remove all unburned pieces of fuse wire from the bomb electrodes; straighten them and measure their combined length in centimeters. Subtract this length from the initial length of 10 centimeters and multiply this burned length by 2.3 calories per cm (for Parr 45C10 Fuse Wire) to obtain the fuse correction.
6772 Calorimetric Thermometer Instruction Manual Remove all unburned pieces of fuse wire from the bomb electrodes; straighten them and measure their combined length in centimeters. Subtract this length from the initial length of 10 centimeters and multiply this burned length by 2.3 calories per cm (for Parr 45C10 Fuse Wire) to obtain the fuse correction. The scale on the fuse wire card can be used to obtain this value directly.
6772 Calorimetric Thermometer Instruction Manual 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. Main Menu Selecting the Main Menu key on any menu will return you to the screen pictured on the right of this page. This key appears in the Escape key location when the main menu is displayed.
6772 Calorimetric Thermometer Instruction Manual Start Preweigh: This key is used to start the sample preweigh process. The user is presented with or prompted for a sample ID. Next, the user is asked to key in the associated sample mass or alternatively the mass is retrieved from a connected balance. Stirrer: On / Off This key provides a convenient way to manually start and stop the calorimeter stirrer motor. The motor must be physically turned on for this function to be active.
6772 Calorimetric Thermometer Instruction Manual Time Units: Toggles between minutes and seconds. Bucket Plot Color: Toggles between: • Red • Green • Yellow • Blue • Magenta • Cyan • White • Black Bucket Max Value: Press this key to access its numeric dialog box to set a maximum bucket value. Jacket Plot Color: Toggles between: (same as Bucket Plot Color, above). Jacket Max Value: Press this key to access its numeric dialog box to set a maximum jacket value.
6772 Calorimetric Thermometer Instruction Manual Jacket Temp. Source: Press this key to display a menu that allows the user to select the source for the jacket temperature used for tests. “Other” Multiplier: Press this key to display the Other Multiplier dialog box, where the user can enter a final multiplier to be used when the reporting units are set to “Other”. Calibrate Touchscreen: This key prompts the user to touch the screen at predefined points in order to facilitate touch screen calibration.
6772 Calorimetric Thermometer Instruction Manual Weight of Fixed Spike: The weight of the fixed spike is entered on sub-menu keyboard. Normally the Calorimetric Thermometer will prompt the user for the weight of the sample and then the weight of the spike. Prompt for Spike Before Weight: When set to ON, the Calorimetric Thermometer will prompt the user for the weight of the sample and the weight of the spike.
6772 Calorimetric Thermometer Instruction Manual Settings Protect: Provides protection for the program options and settings on the menus. If this is turned ON, the user will be warned that enumeration keys are locked when a key is pressed. Enumeration Keys either toggle a value (ON/OFF) or select from a predefined list. This feature is used primarily to protect the instrument settings from accidental changes if one were to inadvertently touch or bump up against the touch screen.
6772 Calorimetric Thermometer Instruction Manual Cold Restart: This is essentially the same as cycling power on the unit. All valid test data will be retained during this cold restart procedure. Calibration Data and Controls Menu Calibration Run Limit: Displays the maximum number of runs that will be included in determining the EE value of a bomb and bucket combination and accesses the sub-menu on which this limit is set. Most test methods suggest 10 tests.
6772 Calorimetric Thermometer Instruction Manual • Process Sigma: In relation to calorimetry, sigma is used as the classification of the instrument. The higher the process sigma the higher the limits for acceptable values for precision control. The Process Sigma of the 6772 will depend on the application. • Temp. Rise High Warning: Sets the high warning limit on the bucket temperature rise. A temperature rise higher than this value will generate a warning message. • Temp.
6772 Calorimetric Thermometer Instruction Manual Name: Enables the operator to assign a unique alpha-numeric label for the bomb ID. The ID can be up to 8 characters. Protect EE Value: Toggles between OFF and ON. When set to OFF, the 6772 automatically updates the EE value as new tests are run. When set to ON, it keeps the EE value protected, whether it has been revised manually via the Manual EE Entry key or calculated by the instrument.
6772 Calorimetric Thermometer Instruction Manual Thermochemical Corrections Menu The Thermochemical Corrections Menu permits three types of fixed corrections for standardization (instrument calibration) runs, and the same three types for determination (test) runs. Pressing the LEFT side of each key toggles the correction ON or OFF. Press the RIGHT side of each key to access the specific numeric dialog box where that fixed value can be set.
6772 Calorimetric Thermometer Instruction Manual Calculation Factors: Accesses the Calculation Factors sub-menu, which provides for setting a number of options for the way the thermochemical corrections are applied. Determination Correction Fixed Fuse Correction: Press this key on the LEFT side to toggle ON or OFF the fixed fuse correction for determination runs.
6772 Calorimetric Thermometer Instruction Manual Calculation Factors Menu Nitric Acid Factor: Ratio of the nitric acid correction when the released energy corresponds to 6318 calories. The default is 1.58 calories per 1000 calories of released energy. Acid Multiplier: This multiplier is the normality of the sodium carbonate used to titrate for the acid correction. The default value of 0.0709 allows for direct entry of the acid correction in calories.
6772 Calorimetric Thermometer Instruction Manual Net Heat/Dry Heat Factors Fixed Hydrogen: ON/OFF and value entry. Fixed Oxygen: ON/OFF and value entry. Fixed Nitrogen: ON/OFF and value entry. Calculate Net Heat of Combustion: ON/OFF. Turn On to have the calorimeter calculate the net heat of combustion. Fixed Moisture as Determined: ON/OFF and value entry. Fixed Moisture as Received: ON/OFF and value entry. Dry Calculation: ON/OFF. Turn on to have the calorimeter calculate the result on a dry basis.
6772 Calorimetric Thermometer Instruction Manual Automatic Sample ID: When set to ON the unit will automatically assign sample identification numbers in accordance with parameters set by the other three keys on this menu. When set to OFF, the user manually enters each sample ID when prompted to do so. Auto Sample ID Prefix: An entry here will be used as a prefix for all sample IDs, if the Automatic Sample ID is set to ON. Press this key to access a submenu for entering an alphanumeric prefix.
6772 Calorimetric Thermometer Instruction Manual Auto Preweigh Controls: Accesses sub-menu, used to automatically assign Sample ID numbers when a series of samples are preweighed ahead of the time they are actually tested. Automatic Preweigh ID: ON/OFF toggle for this feature. Automatic Preweigh ID Prefix: An entry here will be used as a prefix for all pre-weigh sample IDs.
6772 Calorimetric Thermometer Instruction Manual Recalculate Final Reports: When set to ON, causes a recalculation of stored final reports using calibration data and menu settings currently in the Calorimetric Thermometer. When set to OFF, the stored final reports are not affected by the current run. Use New EE Value in Recalculation: When set to ON, any recalculation made will use the most recent EE value in the calculations.
6772 Calorimetric Thermometer Instruction Manual • • • • Data Characters from Balance. This setting is only used when the generic balance format is selected. This value determines the number of numeric data characters (0-9 . + -) to accept. Any additional characters after this value and before the string terminating are discarded. Data Precision. This key allows the user to establish the number of digits to the right of the decimal point that are passed from the balance handler.
6772 Calorimetric Thermometer Instruction Manual Copy Run Data to SD Card: This key copies all test data to a SD memory card inserted into the rear of the calorimeter controller. This feature is used as a means of either archiving data or transferring it to a PC. Copy User Settings to SD Card: This key copies all previously saved user setups to the SD. Copy User Settings From SD Card: This key copies all user setups previously saved to SD back to the calorimeter controller memory.
6772 Calorimetric Thermometer Instruction Manual 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 this instruction manual in order to obtain the maximum benefits from these capabilities. Calorimetry Parameters: This key accesses its sub-menu which allows access to the calorimetry parameters used to automatically sequence a calorimetric test.
6772 Calorimetric Thermometer Instruction Manual Select Data Log Items: Press this key to access the Data Log Items sub-menu, which provides keys for fifteen items that can be individually selected for logging. By default, both the bucket and jacket temperatures are logged. All records are date and time stamped. The most commonly helpful items to log are: D0 - Corrected calorimeter drift rate. Tsum - Accumulated temperature rise. T1 - Extrapolated temperature rise.
6772 Calorimetric Thermometer Instruction Manual View System Info: Press this key to display a screen with current operating system information / statistics such as: • Processes and their associated PIDs • Memory • Mass Storage • Network Press the Print key to print this information. View Instrument Log: Press this key to display a screen with contents of the /tmp/instlog file. It contains a sequential log of the instrument’s processing. Press the Print key to print this log.
6772 Calorimetric Thermometer Instruction Manual CALCULATIONS Corrections Fuse Correction The fuse correction applied by the Calorimetric Thermometer is calculated as: e3 = (fuse value) (Fuse Multiplier) Fuse corrections can be entered when Fixed Fuse in the Thermochemical Corrections menu, is set to OFF. To enter in the fuse correction in cm while using the Parr 45C10 fuse wire, enter a Fuse Multiplier of 2.3 cal/cm. The calorimeter will perform the calculation and provide the correction in calories.
6772 Calorimetric Thermometer Instruction Manual acid value. Total errors of more than 3 calories will seldom occur when using fixed nitric acid corrections. Sulfur Correction In the oxygen rich atmosphere within the bomb, sulfur in the sample is oxidized to sulfur trioxide which combines with water vapor to form sulfuric acid. This liberates additional heat over the normal combustion process which converts sulfur to sulfur dioxide. The sulfur correction removes this excess heat from the calculation.
6772 Calorimetric Thermometer Instruction Manual Fixed Corrections In many cases, fixed values for fuse and acid can be used without introducing a significant error since the corrections are both relatively small and constant. Fixed sulfur corrections can also be used whenever a series of samples will be tested with a reasonably constant sulfur content. Any value set-up as a fixed correction will be automatically applied and the controller will not prompt the user for this value.
6772 Calorimetric Thermometer Instruction Manual Acid Multiplier Calculation: Total acid milliequiv alents - milliequiv alents of H2SO 4 = milliequiv alents of HNO3 (milliequivalents of HNO3)(Hf of HNO3) = calories due to HNO3 formation = 0.0709 Sulfur Correction: e2 = (percent sulfur)(sample mass)(sulfur multiplier)(heat of formation of H2SO4). Acid Correction: In the 6772 there are a number of settings for the acid correction. e1 is the nitric acid portion of the correction.
6772 Calorimetric Thermometer Instruction Manual e1 = [((25)(.0709)) – (2)(1)(.6238)] 14.1 e1 = [(1.7725) – (1.2476)] 14.1 e1 = [.5249] 14.1 e1 = 7.40109 calories When the Acid Correction is set to Fixed Total the value is considered a final value and the operator is not prompted for an acid value when reporting the results. Entered Total: The Acid Correction represents the total base required to titrate the bomb washings (in milliliters). This includes both nitric and sulfuric acid.
6772 Calorimetric Thermometer Instruction Manual ASTM, ISO and Other Methods Current ASTM, ISO, and British Standard Methods differ on their treatment of the nitric and sulfuric acid thermochemical corrections. ASTM Methods call for titrating the bomb washings to determine the total acid present. This is assumed to be all nitric acid with a heat of combustion of -14.1 Kcal per mole. The amount of sulfur is then determined and converted to equivalents of sulfuric acid.
6772 Calorimetric Thermometer Instruction Manual The values for fixed acid and sulfur, which are used in preliminary reports, will reflect a sulfur correction of 0, and a nitric acid correction of 10 calories. Conversion to Other Moisture Bases The calculations described previously give the calorific value of the sample with moisture as it existed when the sample was weighed. For example, if an air-dried coal sample was tested, the results will be in terms of heat units per weight of air-dry sample.
6772 Calorimetric Thermometer Instruction Manual 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 port of the Calorimetric Thermometer. This menu also selects the type of reports that are generated automatically by the Calorimetric Thermometer.
6772 Calorimetric Thermometer Instruction Manual The EDIT key brings up a sub-menu which enables the operator to edit any of the data in the report or add thermochemical corrections to convert preliminary reports to final reports. Final reports can only be edited if Edit Final Reports on the Reporting Controls Menu is turned on. To have the Net Heat of Combustion print as part of preliminary and final reports, go to the Thermochemical Corrections Menu and turn ON Calculate Net Heat of Combustion.
6772 Calorimetric Thermometer Instruction Manual 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.
6772 Calorimetric Thermometer Instruction Manual MAINTENANCE Refer to Manual 204M, Operating Instructions for the 1341 Oxygen Bomb Calorimeter for calorimeter maintenance information. Refer to Manual 205M, Operating Instructions for the 1108 Oxygen Bomb for bomb maintenance information.
6772 Calorimetric Thermometer Instruction Manual 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 selfexplanatory. The following list contains errors that are not necessarily self-evident and suggestions for correcting the error condition. A Misfire Condition Has Been Detected.
6772 Calorimetric Thermometer Instruction Manual substitution can be useful in determining the cause of the problem (probe or electronics). The valid working range of the probe resistance is 1000 to 5000 ohms. A / D Initialization Failed. Shortly after power is applied to the calorimeter controller and the operating system has started, the CPU attempts to read the unique IO board calibration information from the IO board.
6772 Calorimetric Thermometer Instruction Manual TECHNICAL SERVICE Contact Us Should you need assistance in the operation or service of your instrument, please contact the Technical Service Department. Telephone: (309) 762-7716 Toll Free: 1-800-872-7720 Fax: (309) 762-9453 Email: parr@parrinst.com Any correspondence must include the following basic information: 1. 2. 3. 4. The model and serial # of the instrument. Date purchased. Software version(s) shown on the “Software and Hardware Information” page.
6772 Calorimetric Thermometer Instruction Manual PARTS LIST Principal Assemblies in 6772 Calorimetric Thermometer Part Number 1940E A2141E A2154E4 A2140E A2166E A2167E 2147E 1168E2 A719E 1200EEE 1889E 1344DD 139E23 1641E Description Power Supply LCD Transition Board CPU Board I/O Board Cable, I/O to CPU USB Cable, USB Peripheral Touchscreen LCD with Cable Thermistor Probe Cordset, 115V Corset, 220V, EU Plug Film, Display Protection Stylus Fuse Fast/ Act 15 Amp 250V Fuse Fast/ Act 1.
6772 Calorimetric Thermometer Instruction Manual DRAWINGS 6772 Schematic 13-1
6772 Calorimetric Thermometer Instruction Manual Internal Parts View of 6772 Calorimetric Thermometer 13-2
6772 Calorimetric Thermometer Instruction Manual Internal Parts View of 6772 Calorimetric Thermometer Note: 1262DD Capacitor Bracket and 897E Capacitor not shown for clarity.
6772 Calorimetric Thermometer Instruction Manual Internal Parts View of 6772 Calorimetric Thermometer Back Panel of 6772 Calorimetric Thermometer 493E Plug with 3280HC Retainer installed to insulate from live circuits when no motor is attached.
72 Calorimetric Thermometer Instruction Manual TABLES Table 1 – Default Settings Calorimeter Operation Operating Mode Bomb Installed/EE Stirrer Operating Controls Method of Operation Reporting Units Use Spiking Correction Combustion Btu/lb OFF “OTHER” Multiplier 4.
6772 Calorimetric Thermometer Instruction Manual Table 1 - Continued Reporting Controls Report Width Automatic Reporting Auto Report Destination Individual Printed Reports Edit Final Reports Recalculate Final Reports Use New EE Values in Recalculation Communication Controls Printer Printer Type Printer Destination Diagnostics Calorimetry Parameters Tolerance (L) Parameters Preperiod Tolerance (L1) Mis-Fire Tolerance (L2) Dynamic Postperiod Tolerance (L3) Eqlbrm Postperiod Tolerance (L4) Preperiod Stability
6772 Calorimetric Thermometer Instruction Manual Table 2 – ISO & BSI Method Settings Page Line Acid Correction (STD) Thermochemical Corrections Fixed Sulfur STD Acid Correction (DET) Calculations Factors Fixed Sulfur DET Acid Multiplier Sulfur Value is Percent Sulfur Multiplier Use Offset Correction Offset Value 14-3 Setting Entered HNO3 Off Entered HNO3 Off Value 13 7 13 7 0.154 Off 0.1 On -43.
PARR INSTRUMENT COMPANY 211 Fifty - Third Street Moline, Illinois 61265 USA 309 / 762-7716 800 / 872-7720 Fax 309 / 762-9453 http://www.parrinst.com parr@parrinst.
