Operating Instruction Manual 534M 6400 Calorimeter
6400 Calorimeter Instruction Manual TABLE OF CONTENTS TABLE OF CONTENTS ................................................................................................1-1 PREFACE ......................................................................................................................1-1 Scope .........................................................................................................................1-1 Purpose........................................................................
6400 Calorimeter Instruction Manual Operating Controls Menu ...........................................................................................5-3 Program Information and Control Menu.....................................................................5-6 Calibration Data and Controls Menu ..........................................................................5-8 Thermochemical Corrections Menu .........................................................................
6400 Calorimeter Instruction Manual PREFACE Scope This manual contains instructions for installing and operating the Parr 6400 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.
6400 Calorimeter Instruction Manual Purpose Heats of combustion, as determined in an oxygen bomb calorimeter such as the 6400 Isoperibol Calorimeter, are measured by a substitution procedure in which the heat obtained from the sample is compared with the heat obtained from a standardizing material. In this test, a representative sample is burned in a high-pressure oxygen atmosphere within a metal pressure vessel or “bomb”.
400 Calorimeter Instruction Manual 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.
6400 Calorimeter Instruction Manual INSTALLATION Note: Some of the following manual sections contain information in the form of warnings, cautions and notes that require special attention. Read and follow these instructions carefully to avoid personal injury and damage to the instrument. Only personnel qualified to do so, should conduct the installation tasks described in this portion of the manual. Each Parr 6400 Calorimeter was completely assembled and thoroughly tested prior to shipment.
6400 Calorimeter Instruction Manual tighten slightly with a wrench. Smaller tube sizes (up to 3/16” or 4mm) take less tightening to reach the original position than larger tube sizes. The type of tubing and the wall thickness also has an effect on the amount of tightening required. Plastic tubing requires a minimal amount of additional tightening while heavy wall metal tubing may require somewhat more tightening.
6400 Calorimeter Instruction Manual Figure 1 - 6400 Calorimeter Back Panel - Label Water Connection Remove the cap plug on the water filling elbow and fill the internal reservoir tank with water having a total hardness of 85 ppm or less, until the water level is at the bottom of the filling elbow. The calorimeter water tank will initially accept about 2 liters.
6400 Calorimeter Instruction Manual Fill the external rinse tank with about 16 liters of distilled water through the large opening at the top of the tank. The cover for this opening is removed by lifting up on the handle, pushing down on the lid, tilting and removing. Replace and close the cover after filling. The two connections between the calorimeter and the 1576 Rinse Tank should be made with two pieces of 1/8” nylon pressure hose (HX0012TB024).
6400 Calorimeter Instruction Manual Note: A hissing sound will occur while the rinse tank is being pressurized. This is normal. Adjust the pneumatic supply regulator to 80 psig as needed. During extended periods of inactivity, close the tank valve to prevent depleting the tank in the event of a leak. Close the tank valve prior to removing the regulator when changing tanks. Do not use oil or combustible lubricants in connection with any part of the oxygen filling system.
6400 Calorimeter Instruction Manual Table 1 - 6400 Calorimeter Serial Ports Pin-Out 9 pin D Connector Pin # Description 2 3 4 5 6 7 8 Received Data Transmitted Data Direction (6400 – External Device) Í Î Signal Ground ÍÎ Ready to Send (RTS) Clear to Send (CTS) Î Í The RS232 balance port is a female port whereas the RS232 printer port is a male port. The 6400 Calorimeter is also equipped with an RJ45 Ethernet port for connection to a computer.
6400 Calorimeter Instruction Manual Multiple Alternate Configurations Printer Connections The printer port settings are on the Communication Controls Menu: Printer Port Communications Menu. The default parameters for the 6400 are set up for use with the Parr 1757 Printer. Table 1 identifies and describes the pin-out for the RS-232 port. Balance Connections The 6400 Calorimeter supports input from the multiple balance types.
6400 Calorimeter Instruction Manual Field ID space data space g CR LF Mettler 011/012 Interface The ID field must contain “S_” to indicate a stable mass. The data field contains the current mass, right justified, with a decimal point. The balance should be configured to send continuously. Sartorious Interface The polarity field must contain either a “+” or a space. Leading zeros in the data field are blanked, except for the one to the left of the decimal point.
6400 Calorimeter Instruction Manual Computer Connections If the 6400 Calorimeter is to be connected to a computer, the Ethernet connection should be used. Test data can be transferred to an Ethernet network connected computer using the FTP File Transfer Protocol. First, you must know the IP address of the network-connected calorimeter. The network DHCP (Dynamic Host Configuration Protocol) server provides this address shortly after the calorimeter is turned on.
6400 Calorimeter Instruction Manual The following screenshot illustrates the contents of the calorimeter 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.
6400 Calorimeter Instruction Manual The calorimeter 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 calorimeter. Clicking on the Sample Data tab displays a list of reports currently in the instrument memory.
6400 Calorimeter Instruction Manual Clicking on any given report will provide a display similar to the following: 2-12
6400 Calorimeter Instruction Manual QUICK START 1. Turn on the heater and pump in the Calorimeter Operation menu. Allow at least 20 minutes for the calorimeter to warm up. 2. Initiate a pretest to run the calorimeter through the fill and cool/rinse cycles. This function is used to pre-condition the calorimeter if it has been sitting idle for an extended period of time (greater than 15 minutes). 3. Prepare and weigh the sample to 0.0001g. 4.
6400 Calorimeter 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.
6400 Calorimeter Instruction Manual Control Keys There are five control keys which always appear in the right column of the primary displays. These keys are unavailable when they are gray instead of white. 1. Escape. This key is used to go up one level in the menu structure. 2. Main Menu. This key is used to return to the main menu touch screen from anywhere in the menu structure. 3. Start. This key is used to start a test. 4. Report.
6400 Calorimeter Instruction Manual To re-load the user default setting, go to the Program Info and Control Page, User/Factory Settings, Re-load User Default Settings, and YES. Sample Preparation Sample Size To stay within safe limits, the bomb should never be charged with a sample which will release more than 8000 calories when burned in oxygen. The initial oxygen pressure is set at 30 atmospheres (450 psig).
6400 Calorimeter Instruction Manual Sample Types Because of the difference in combustion characteristics of the many different materials which may be burned in an oxygen bomb, it is difficult to give specific directions which will assure complete combustions for all samples.
6400 Calorimeter Instruction Manual who intend to test these materials are urged to select the 1138CL Bomb. These bombs are 250 mL in volume and are rated to a maximum working pressure of 2000 psi. The bombs are hydrostatically tested to 3000 psi and the sample range is ~1g or 5000 – 8000 calories. Explosives and High Energy Fuels Materials which release large volumes of gas which detonate with explosive force or burn with unusually high energy levels, should not be tested in this calorimeter.
6400 Calorimeter Instruction Manual 4. Set the cup in the capsule holder and arrange the auxiliary fuse so that it touches the center of the tape disc. 5. Just before starting the test, prick the disc with a sharp needle to make a small opening which is needed to prevent collapse of the disc when pressure is applied. 6. Fill the bomb with the usual oxygen charging pressure. 7. The calorimeter will fire the bomb and complete the test in the usual manner.
6400 Calorimeter Instruction Manual When superior corrosion resistance is needed, the Platinum Rhodium 43A5 Capsule is required. Test Process Loading the sample Prepare and weigh the sample to 0.0001g. Gently tap capsules that contain powdered samples to compact the material. (Pellets are easier to handle than loose samples and they burn slower in the bomb, thereby reducing the chances for incomplete combustion). Carefully place the capsule into the capsule holder.
6400 Calorimeter Instruction Manual Notice that the bomb head grounding lug extends beyond the outside diameter of the bomb head. A slot for this lug is cut into the top of the calorimeter bucket which holds the bomb cylinder. Position this lug approximately 20 degrees to the operators right and slide the head into the cylinder and push it down as far as it will go.
6400 Calorimeter Instruction Manual 2. The water fill solenoid opens and water is pumped from the internal tank into and through the bucket that surrounds the bomb. Overflow from the bucket is returned to the closed water tank. Because the jacket and bucket are both filled with water from the closed water tank, initial equilibrium will be reached quickly. 3. The oxygen fill solenoid is opened and oxygen is added slowly to the bomb to bring its pressure to approximately 30 atm.
6400 Calorimeter Instruction Manual continues to circulate from the closed water system through the jacket surrounding the bucket. 2. The oxygen filling valve closes and the pressure in the filling line is vented. The automatic check valve at the top of the bomb closes and isolates the bomb from the oxygen filling line. 3. The controller monitors the operating temperature until it confirms that the initial equilibrium has been established.
6400 Calorimeter Instruction Manual Cool / Rinse At the completion of the post-period, the rinse and cool sequence begins. Figure 8 - Rinse & Cool Flow Diagram 1. Chilled water is circulated through the bucket to cool the bomb to the starting temperature. 2. The release valve in the bottom of the bomb is opened and the residual pressure is released through the bomb exhaust line. 3.
6400 Calorimeter Instruction Manual Note: Several rinse patterns may be configured by the user to meet various operational and analytical requirements. 4. The bomb is filled one more time with oxygen to help flush the water residue from the interior of the bomb. Drain At the completion of the bomb rinse sequence, the drain sequence begins.
6400 Calorimeter Instruction Manual Figure 9 - Drain Flow Diagram The water in the bucket is drained out of the bucket and routed to the drain connection. Once the bucket is drained, the calorimeter may be opened to remove the bomb head and load the next sample. The test result will then print or be displayed.
6400 Calorimeter 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 Escape Key: Selecting the Escape key on any menu will return you to the menu one level up. Main Menu Key: Selecting the Main Menu key on any menu will return you to the screen pictured on the right of this page.
6400 Calorimeter Instruction Manual Start Preweigh: This key is used to start the sample pre-weigh 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. Heater and Pump: The heater and pump must only be turned on after the calorimeter water tank is filled with water.
6400 Calorimeter Instruction Manual Bucket Min Value: Press this key to access its numeric dialog box to set a minimum bucket value. Jacket Plot Symbol: (same as Bucket Plot Symbol, above). 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 X-axis Time Units: Toggles between minutes and seconds.
6400 Calorimeter Instruction Manual Spiking Correction: Accesses the Spike Controls sub-menu: “Spiking” is the addition of material, such as benzoic acid or mineral oil, to samples which are difficult to burn in order to drive the combustion to completion. Use Spiking. When set to ON, the calorimeter will prompt for the weight of the spike added and will compensate for the heat of combustion in the calculations. Heat of Combustion of Spike.
6400 Calorimeter Instruction Manual Reset Rinse Tank Counter. Resets the counter when the rinse tank has been refilled. This counter must be reset after the rinse tank is refilled. Rinse Time. This value establishes the time that the rinse water solenoid is turned ON for each rinse cycle. When the rinse water solenoid is ON, distilled water from the rinse tank is pumped, under pressure, into the bomb cylinder. This rinses the cylinder walls and the bomb head.
6400 Calorimeter Instruction Manual 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 Calorimeter through the installed operating languages. Program Information and Control Menu Date: Displays current date and accesses sub-menu on which date is set in (YY/MM/DD) format.
6400 Calorimeter Instruction Manual User Setup ID Used to enter a unique identifier for recalling user settings. Parr offers a unique program within the 6400 identified as “63-FAST”. The program will “overlay” the factory settings and shorten the run time by approximately 2 minutes however the user should be aware that a loss of precision will occur. Reload Factory Default Settings: Used to erase all of the settings and restore the factory default settings.
6400 Calorimeter Instruction Manual 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 submenu on which this limit is set. Most test methods suggest 10 tests. Tests in excess of the most recent ones used are still available but are not used in the calculation of the EE value.
6400 Calorimeter Instruction Manual Bomb 1: Leads to sub-menu, Bomb 1. Displays standardization information for bomb and bucket combinations. While only one bomb and bucket is installed in the calorimeter at a time, a spare may be used for servicing and for more rapid turn-around. The respective EE values for each bomb can be stored in memory. Note: For rapid turn around between tests, the user may wish to use an extra head. Each head should be assigned a bomb ID.
6400 Calorimeter Instruction Manual Print Standardization Runs: This key will print all of the tests that have been incorporated into the calculated EE value. This will be helpful in evaluating a series of tests which fail to produce a satisfactory EE value and relative standard deviation. Reset Bomb Fire Count: After bomb service, press this key to reset the fire count to zero.
6400 Calorimeter 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.
6400 Calorimeter Instruction Manual Fixed Acid Correction: Press this key on the LEFT side to toggle ON or OFF the fixed acid correction for determination runs. Press it on the RIGHT side to access the Fixed Acid numeric dialog box on which the value can be set. Fixed Sulfur Correction: Press this key on the LEFT side to toggle ON or OFF the fixed sulfur correction for determination runs. Press it on the RIGHT side to access the Fixed Sulfur numeric dialog box on which the value can be set.
6400 Calorimeter Instruction Manual Sulfur Value is Percent: When set to ON, the sulfur value is being entered as weight percent sulfur. If another system is to be used, this must be turned OFF and the sulfur multiplier set accordingly. Sulfur Multiplier: Values entered by the user to be used for the sulfur correction are multiplied by this value to get the product into units of milliequivalents. The default number (0.6238) requires that the sulfur value be entered in weight percent.
6400 Calorimeter Instruction Manual Moisture Multiplier: Press to access the Moisture Multiplier numeric dialog box and set the value. This value is associated with the net heat calculation. It is related to the heat of vaporization of water. Data Entry Controls Menu Prompt for Bomb ID: Toggles ON or OFF. In the ON position the controller will prompt for a Bomb ID (1-4) when a test is started.
6400 Calorimeter Instruction Manual 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 sub-menu 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.
6400 Calorimeter Instruction Manual Reporting Controls Menu Report Width: Toggle this key to set the column width of the printer to either 40 or 80 columns. Select 40 when the 1757 Printer is used. Automatic Reporting: Toggles the automatic reporting ON/OFF. When ON, preliminary reports will be generated at the conclusion of the test and final reports will be generated as soon as all of the thermochemical corrections are available. When OFF, reports will only be generated by selecting the Report key.
6400 Calorimeter Instruction Manual Printer Port (RS232): Accesses sub-menu, Printer Port Communications. Sets the communication parameters for the RS232 ports used for the printer port. Standard options for data bits, parity, stop bits, handshaking, baud rate and balance type are provided to match any devices that might be connected to these ports. • 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.
6400 Calorimeter Instruction Manual • • • • • • • • 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. Data Characters from Balance.
6400 Calorimeter Instruction Manual Further information on establishing communications for the Printer Port, Balance Port, Network Interface, Bar Code Port and other Network Data Devices can be found in the Installation section of this manual. 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.
6400 Calorimeter Instruction Manual 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. This indicates that it is selected. Multiple files throughout the list can be selected in this fashion. Extend Sel: This key selects all files between the last file selected and the file that is highlighted in blue.
6400 Calorimeter Instruction Manual Data Logger: Displays ON/OFF status and accesses the Data Logger Controls Menu for setting the specific logging controls. Data Logger: This key toggles the data logging function ON / OFF. Data Log Interval: This key displays the interval of which the selected data is logged. The interval in seconds is defined in the Select Data Items sub-menu (normally 12 seconds). This roughly matches the update interval for the bucket temperature.
6400 Calorimeter Instruction Manual View System Log: This key accesses its sub-menu which displays the contents of /flash/log/messages. This file is used primarily to log application program debug messages. Press the Print key to print these messages. User Defined Functions: This key leads to a sub-menu that offers five special purpose user/ factory definable function keys. Combine Det. Reports: Pressing this key combines all determination reports into a single file named /tmp/bigdetfile.txt. Combine Std.
6400 Calorimeter Instruction Manual I/O Diagnostics: Press this key to display the I/O Diagnostics sub-menu, which allows the user to manipulate digital outputs for troubleshooting. The I/O Diagnostics screen is used to display the digital outputs at a basic level for troubleshooting. Both the bucket and jacket temperatures are also displayed on this screen. Any output can be selected using the left and right arrow keys. The selected output is turned ON (1) or OFF (0) using the 1 and 0 keys.
6400 Calorimeter Instruction Manual CALCULATIONS Corrections Fuse Correction There are two components to the fuse correction in the 6400 Calorimeter: The heat introduced by heating the wire used to ignite the cotton thread. The heat of combustion of the cotton thread used to ignite the sample. e3 = (fuse value) (fuse multiplier) The semi-permanent heating wire is heated by dissipating an electrical charge from a capacitor.
6400 Calorimeter Instruction Manual This factor is added to the calculations when Spike Controls, Use Spiking is set to ON. The Heat of Combustion of the spiking material is entered as calories per gram. The calorimeter will prompt the user to enter the weight of spiking material. Fixed spikes can also be used. To do this, set Use Fixed Spike to ON and enter the mass of the spike (Weight of Fixed Spike key).
6400 Calorimeter Instruction Manual Manual Entry During the reporting process, the controller will prompt the user to enter the following values: • Fuse Correction Key in the Fuse/Heat Wire Correction and press the ENTER key. The default setting for this value is to be entered in calories. • Acid Correction Key in the Acid Correction and press the ENTER key. The default setting for this value is to be entered in milliliters of standard alkali required to titrate total acid or calories.
6400 Calorimeter Instruction Manual Heat of formation of sulfuric acid (from SO2) is 36.1 calories / milliequivalent. Sample mass is the mass of sample burned in the bomb (grams). Sulfur multiplier is multiplied by the product of the user entered sulfur value and the sample mass to arrive at the number of milliequivalents of sulfuric acid in the bomb washings.
6400 Calorimeter Instruction Manual Example 2: The following assumptions are made and outlined in D240. 1) The acid value is ALL nitric 2) The concentration of the titrant used is 0.0866M 3) 1 calorie (I.T.) is equal to 4.1868 Joules 4) The heat of formation of HNO3 is 57.8 kJ/mol 5) The heat of formation of H2SO4 is 301.4 kJ/mol The calorimeter must be set accordingly.
6400 Calorimeter 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.
6400 Calorimeter 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.
6400 Calorimeter Instruction Manual REPORTS The 6400 Calorimeter 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 RS232 printer port of the calorimeter. This menu also selects the type of reports that are generated automatically by the calorimeter. There are two kinds of reports: Preliminary and Final.
00 Calorimeter Instruction Manual The DESEL ALL key is used to cancel the current selection of files. To bring the selected report or series of reports to the display, press the DISPLAY key. To send the reports to the printer press the PRINT key. 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.
6400 Calorimeter Instruction Manual MEMORY MANAGEMENT The 6400 Calorimeter 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 sub-menu. The RUN DATA FILE MANAGER key leads to a listing of the files.
6400 Calorimeter Instruction Manual MAINTENANCE Note: Some of the following manual sections contain information in the form of warnings, cautions and notes that require special attention. Read and follow these instructions carefully to avoid personal injury and damage to the instrument. Only personnel qualified to do so, should conduct the maintenance tasks described in this portion of the manual.
6400 Calorimeter Instruction Manual 2. Use a non-metallic object, such as the rounded corner of a plastic credit card, to simply pry the seal from its groove. Smaller diameter seals usually require a different approach. A portion of the seal should be carefully pulled, not pried, from the groove with a small pair of pliers or a hemostat. The exposed portion of the seal can then be cut, or pulled further to remove the seal. The pliers or hemostat should never contact the sealing surface, only the seal.
6400 Calorimeter Instruction Manual 50 to 100 Test Maintenance Replace the heating wire, with 2” of 840DD2. Wind the wire 360 degrees clockwise around screws. Clean the 986DD Electrode Contact Pins with a mild abrasive, such as a pencil eraser. Clean the bomb head electrode points in a similar fashion and tighten the screws holding the heating wire in place. 500 Test Maintenance Clean the ignition contacts. Under normal usage Parr oxygen bombs will give long service if handled with reasonable care.
6400 Calorimeter Instruction Manual 7. Remove the cylinder spacer, 1141DD, which sits on top of the snap ring, 1137DD. 8. Remove the snap ring that retains the cylinder insert in the release mechanism at the bottom of the air can. Withdraw both the insert and the release pin as a unit using needle nose pliers. 9. If present, remove any scoring on the 966DD2 release pin, above the smaller o-rings, with crocus cloth.
6400 Calorimeter Instruction Manual TROUBLESHOOTING Bomb Exhaust Troubleshooting The bomb exhaust and sealing is controlled by movement of the 966DD2 piston inside of the 1140DD bomb seal/release cylinder. This assembly is mounted on the bottom of the calorimeter air can. The piston is driven to the up position (bomb exhaust) by applying oxygen at 30 atm to the 1/8 male connector (344VB). The piston is driven down (bomb seal) by applying pressure to the 376VB elbow.
6400 Calorimeter Instruction Manual Confirm function of the 966DD2 piston In order to reduce the amount of time it takes to duplicate and troubleshoot this type of situation, the I/O diagnostics can be used to pressurize and exhaust the bomb without having to run lengthy combustion or pre-tests. WARNING: This screen allows unconditional and arbitrary output control for testing purposes. Be aware that all user and instrument protection is disconnected while on this screen.
6400 Calorimeter Instruction Manual Jacket Temperature Troubleshooting The jacket temperature is monitored with the use of a thermistor installed in the A1448DD temperature control assembly. This assembly is heated by a heater cartridge, A1459DD. In the Diagnostics Menu, select Instrument Monitor. If the heater PID is ON and reading 100%, yet the jacket is at ambient temperature, check the following possible causes.
6400 Calorimeter Instruction Manual A Preperiod Timeout Has Occurred The calorimeter has failed to establish an acceptable initial temperature, prior to firing the bomb, within the time allowed. Possible causes for this error are listed below: • • • A bomb leak Poor bucket stirring Lid not tight The Current Run Has Aborted Due To Timeout The calorimeter has failed to establish an acceptable final temperature within the time allowed.
6400 Calorimeter Instruction Manual You Have Exceeded the Run Data File Limit (1000 Files) The memory set aside for test runs has been filled. Use the memory management techniques to clear out non-current tests. Bomb EE Standard Deviation Warning The relative standard deviation for the calibration runs in memory for the indicated bomb exceeds the preset limit. Sample Weight Warning The entered sample mass exceeds the value entered via the Sample Weight Warning Above key on the Data Entry Controls page.
6400 Calorimeter 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.
6400 Calorimeter Instruction Manual PARTS LIST Principal Assemblies in Calorimeter Item Description Oxygen Combustion Vessel 1138/1138CL Power Supply, 24V 1795E Power Supply, 5/12V 1796E Capacitor, Ignition 897E Controller Assembly A1250DD Oxygen Solenoid Assembly A1251DD Water Solenoid Assembly A1447DD Temp Control Sub-Assy A1448DD Water Chiller Assembly A1449DD Pump Assembly Circulating 115V A1254DDEB Pump Assembly Circulating 230V A1254DDEE Propeller Assembly, stirrer A1255DD Tank, Water (A1435DD / 6400)
6400 Calorimeter Instruction Manual A1457DD Accessory / Installation Kit Parts List Item Description Container, PP 10L Foldable 231C2 Benzoic Acid Pellets 100 Gram Bottle O-Ring, 3415 Pliers for Snap Ring 356HCW Capsule, SS 43AS Lube/Sealant 811DD Heating Wire 840DD2 Ignition Thread, 4” 845DD2 Cutter, Plastic Tubing 876DD Forceps 1005DD Waste Tube Assembly A1006DD Bomb Head Support Stand A38A 1/32 Socket Screw Key TX03SK 9/64 Socket Screw Key TX14SK In-line Filter 149C LCD Stylus 1344DD LCD Screen Protector
6400 Calorimeter Instruction Manual A1266DD Cover Assembly Parts List Item Description Contact Pin Assembly Pin Contact 986DD Block Contact Pin 987DD Spring Compression 988DD Snap Ring External .219” 989DD Bushing 0.
6400 Calorimeter Instruction Manual DRAWINGS Figure 10 - 1138 Parts Diagram 13-1
6400 Calorimeter Instruction Manual 1138 Parts Diagram Key Key No.
6400 Calorimeter Instruction Manual Figure 11 - 6400 Cutaway Right 13-3
6400 Calorimeter Instruction Manual Figure 12 - 6400 Cutaway Left 13-4
6400 Calorimeter Instruction Manual Figure 13 - 6400 Cover Open 13-5
6400 Calorimeter Instruction Manual Figure 14 - A1250DD Control Schematic 13-6
6400 Calorimeter Instruction Manual Figure 15 - A1251DD Oxygen Solenoid Assembly Figure 16 – A1447DD Water Solenoid Assembly 13-7
6400 Calorimeter Instruction Manual Figure 17 – A1435DD Rinse Valve Assembly 13-8
6400 Calorimeter Instruction Manual Figure 18 - 6400 Internal Plumbing Diagram 13-9
6400 Calorimeter Instruction Manual Figure 19 - 6400 Water Tank and Jacket Cooling Solenoid 13-10
6400 Calorimeter Instruction Manual Figure 20 – A1455DD Propeller Assembly Apply thread sealant (Locktite or equivalent) to set screw in 1242DD2 pulley before installing.
6400 Calorimeter Instruction Manual Figure 22 - A1268DD Stirrer motor and Mount 13-12
6400 Calorimeter Instruction Manual Figure 23 – 6400 Bucket Assembly 13-13
6400 Calorimeter Instruction Manual Figure 24 - 6400 Air Can Assembly, Cutaway Left 13-14
6400 Calorimeter Instruction Manual Figure 25 - Air Can Assembly, Cutaway Front 13-15
6400 Calorimeter Instruction Manual Figure 26 - A1450DD Bomb Head Assembly, View 1 13-16
6400 Calorimeter Instruction Manual Figure 27 - A1450DD Bomb Head Assembly, View 2 13-17
6400 Calorimeter Instruction Manual Figure 28 – A1050DD Rinse Collection Assembly 13-18
6400 Calorimeter Instruction Manual Figure 29 - Wiring Diagram 13-19
6400 Calorimeter Instruction Manual Figure 30 - Wiring Diagram 13-20
6400 Calorimeter Instruction Manual Figure 31 – Fuse Diagram 13-21
6400 Calorimeter Instruction Manual TABLES Table 2 - Default Settings Calorimeter Operation Operating Mode Bomb Installed/EE Heater and Pump Calibration Data & Controls Calibration Run Limit EE Max Std Deviation Heat of Combustion of Standard Bomb Service Interval Use Bomb Determination 1/940 OFF Operating Controls Method of Operation Reporting Units Use Spiking Correction Dynamic btu/lb OFF “OTHER” Multiplier 4.
6400 Calorimeter Instruction Manual Table 3 - Default Settings Data Entry Controls Prompt for Bomb ID Weight Entry Mode Acid Entry Mode Hydrogen Entry Mode Auto Sample ID Controls Sample Weight Warning above Spike Weight Entry Mode Sulfur Entry Mode Moisture Entry Mode Auto Preweigh Controls ON Touch Screen Touch Screen Touch Screen ON 2.
6400 Calorimeter Instruction Manual Table 4 - ISO & BSI Method Settings Page Thermochemical Corrections Calculation Factors Line Fixed Acid STD Fixed Sulfur STD Fixed Acid DET Fixed Sulfur DET Acid is Nitric Only Acid Multiplier Sulfur Value is Percent Sulfur Multiplier User Offset Correction Offset Value 14-3 Setting Off Off Off Off On 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.