587M 6400 Automatic Isoperibol Calorimeter Operating Instruction Manual For models produced after October 2010
6400 Table of Contents Preface 4 Scope 4 Related Instructions 4 Purpose 4 Explanation of Symbols 5 Safety Information 5 Intended Usage 5 General Specifications 6 Environmental Conditions 6 Closing the bomb 22 Cool/Rinse 26 Drain Fill Cycle 23 Pre-Period 24 Bomb Firing 25 Post-Period 25 Chapter 4 28 Provisions for Lifting and Carrying 6 Menu Descriptions 28 Cleaning & Maintenance 6 Main Menu 28 Calorimeter Operation Menu 28 Chapter 1 8 Installation 8 Environment
Table of Contents Chapter 5 46 Chapter 10 70 Reports Maintenance 46 Reports 46 70 Inspection of Critical Sealing Surfaces 70 Bomb Removal 70 Chapter 6 48 Standardizations 48 Standardizing the Calorimeter 48 Standard Materials 48 Automatic Statistical Calculations 48 Chapter 7 52 Calculations 52 Calculating the Heat of Combustion 52 General Calculations 52 Thermochemical Corrections 52 ASTM and ISO Methods Differ 53 Thermochemical Calculation Details 54 Acid and Sulfur Correc
6400 Table of Contents Figures Figure 1-1 Swagelok Tube Fittings Figure 1-2 6400 Calorimeter Back Panel Figure 1-3 6400 External Plumbing Figure 1-4 6400 Calorimeter Peripherals Figure 1-5 Multiple Alternate Configurations Figure 3-1 Volatile Sample Technique Figure 3-2 Cotton Thread Assembly Figure 3-3 Bucket Fill Flow Diagram Figure 3-4 Pre-Period/Post-Period Flow Diagram Figure 3-5 Rinse & Cool Flow Diagram Figure 3-6 Drain Flow Diagram Figure 14-1 1138 Parts Dia
Preface Preface Related Instructions Scope This manual contains instructions for installing and operating the Parr 6400 Calorimeter. For ease of use, the manual is divided into 15 chapters. 1. Installation 2. Quick Start 3. Operation 4. Menu Descriptions 5. Reports 6. Standardizations 7. Calculations 8. Computer Communications 9. Memory Management 10. Maintenance 11. Troubleshooting 12. Technical Service 13. Parts Lists 14. Drawings 15.
6400 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.
Preface General Specifications Provisions for Lifting and Carrying Electrical Ratings 120VAC, 5.0 Amps. 50/60 Hz 240VAC, 3.0 Amps. 50/60 Hz Before moving the instrument, disconnect all connections from the rear of the apparatus. Lift the instrument by grabbing underneath each corner.
6400 Notes www.parrinst.
1 Installation Chapter 1 Installation Figure 1-1 Swagelok Tube Fittings 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.
6400 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. In general, the nut only needs to be tightened about 1/8 turn beyond finger tight where the ferrule seats in order to obtain a tight seal. Over tightening the nut should be avoided.
1 Installation Figure 1-2 6400 Calorimeter Back Panel 10 Parr Instrument Company
6400 Installation 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. Fill the external rinse tank with about 16 liters of distilled water through the large opening at the top of the tank.
1 Installation Gas Connection Bomb Exhaust Connections Make the connections to the oxygen supply at this time. Refer to Figure 1-3. 1/8” O.D. nylon pressure hose (HX0012TB024) is used to connect the oxygen supply. The inlet connection incorporates a flow restrictor just behind the inlet connection. When making the oxygen connection, a back-up wrench should be placed on the restrictor to insure a secure connection and to prevent over tightening the flow restrictor.
6400 Communication Connections There is a Universal Serial Buss (USB) port at the rear of the calorimeter. The USB port is used to connect to external devices such as a printer or balance. Multiple devices can be attached by installing a USB hub. The 6400 Calorimeter is also equipped with an RJ45 Ethernet port for connection to a computer.
1 Installation Figure 1-4 6400 Calorimeter Peripherals Figure 1-5 Multiple Alternate Configurations 14 Parr Instrument Company
6400 1 Notes www.parrinst.
2 Quick Start Chapter 2 Quick Start Initial Fill When you first fill the calorimeter with water the main reservoir will be filled. There is also a cooling water reservoir that is filled from the main reservoir. Once the calorimeter has been filled with water and all external connections made: 1. Turn on the calorimeter. 2. Once at the Main Menu go to the Calorimeter Operation screen and turn ON the heater and pump. Water should start to circulate in the tubing. chances for incomplete combustion). 5.
6400 2 Notes www.parrinst.
3 Operation Chapter 3 value. Some keys lead to multiple choices. Always clear the current value before entering a new value. Once entered the screen will return to the previous menu and the new value will be displayed in the lower right corner of the key. 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. 4. Data Displays.
6400 Operation Programming Sample Preparation The program in the 6400 Calorimeter can be extensively modified to tailor the unit to a wide variety of operating conditions, reporting units, laboratory techniques, available accessories and communication modes. In addition, the calculations, thermochemical corrections and reporting modes can be modified to conform to a number of standard test methods and procedures.
3 Operation combustions. If moisture is to be added to retard the combustion rate, drop the water directly onto the loose sample or onto a pellet after the sample has been weighed. Then let the sample stand to obtain uniform distribution. Low volatile samples with high water content, such as urine or blood, can be burned in an open capsule by absorbing the liquid on filter paper pulp or by adding a combustion aid, such as ethylene glycol.
6400 Operation Volatile Sample Holders Volatile samples are defined as one with an initial boiling point below 180 ºC. Volatile samples can be handled in a Parr 43AS Alloy Capsule which has a sturdy wall with a flat top rim. These holders can be sealed with a disc of plastic adhesive tape prepared by stretching tape across the top of the cup and trimming the excess with a sharp knife.
3 Operation Combustion Capsules Non-volatile samples to be tested in Parr oxygen bombs are weighed and burned in shallow capsules measuring approximately 1” diameter and 7/16” deep. These are available in stainless steel, fused silica, fused quartz, and platinum alloyed with 3-1/2% rhodium. Stainless steel capsules (43AS) are furnished with each calorimeter.
6400 Operation Fill Cycle Once the calorimeter is started and the cover is closed, the fill sequence begins. Figure 3-3 Bucket Fill Flow Diagram 1. The calorimeter checks the bomb ignition circuitry for continuity. 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.
3 Operation Pre-Period At the completion of the fill sequence, the pre-period begins. Figure 3-4 Pre-Period/Post-Period Flow Diagram 1. The water fill solenoid valve closes and isolates the water in the bucket from the rest of the system. Water within this bucket is circulated by the stirrer. Water 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.
6400 Bomb Firing Once the initial equilibrium is confirmed, the controller initiates the firing sequence. There are no changes to the circulation pattern, as shown in Figure 3-4, from the pre-period through the bomb firing and post-period. A warning of short beeps is sounded indicating the bomb is about to be fired. Operation Post-Period A minimal temperature rise will confirm that the sample has ignited. After this verification, the postperiod begins. See Figure 3-4. 1.
3 Operation Cool/Rinse At the completion of the post-period, the rinse and cool sequence begins. Figure 3-5 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. Once the excess oxygen is vented, the bomb rinse water from the rinse water tank is admitted through the bomb rinse solenoid valve and the check valve at the top of the bomb.
6400 Operation Drain At the completion of the bomb rinse sequence, the drain sequence begins. Figure 3-6 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. www.parrinst.
4 Menu Descriptions Chapter 4 Menu Descriptions Calorimeter Operation Menu The Calorimeter will normally be operated from the Calorimeter Operation Menu, although tests can always be started from any menu screen. 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.
6400 Temperature vs. Time Plot Menu Descriptions Bucket Plot Symbol: Toggles between »» No Point »» Small Dot »» Round »» Square »» Up Triangle »» Down Triangle »» Diamond Bucket Min Value: Press this key to access its numeric dialog box to set a minimum bucket value. Jacket Plot Symbol: Toggles between (same as Bucket Plot Symbol, above).
4 Menu Descriptions Operating Controls Menu Method of Operation: Offers an operating mode of either dynamic or equilibrium. In most cases, the dynamic mode with its curve matching capability will save approximately 3-4 minutes per test and will produce the same operating precision as the slower equilibrium mode. Reporting Units: Offers a choice of BYU/lb, cal/g, J/kg, or MJ/kg for the reporting units. A user selected set of reporting units may be chosen by selecting “other”.
6400 Bomb Rinse Tank Controls Menu Descriptions Rinse Flush Time: This value is used to establish a time between rinse cycles. During this time the rinse solenoid is turned OFF. This off time permits the rinse water to drain out before the next rinse cycle begins. The factory default value is 2s. Clear Time: This time value is used to establish a post-rinse oxygen filling time for the bomb. This step is used to clear the lines and valves of any residual rinse water prior to the next test.
4 Menu Descriptions Program Information and Control Menu Software and Hardware Info: This screen displays important information such as the main software version, I/O board information, CPU information, and IP address assigned. Software & Hardware Info Date & Time: Accesses a sub-menu to set the current date and time. Date: Displays current date and accesses sub-menu on which date is set in (YY/MM/DD) format. Time: Displays current time and accesses submenu on which time is set in (HH:MM) format.
6400 User/Factory Settings: This key leads to a submenu that allows the user to save or recall user defined instrument settings. Additionally, factory pre installed settings supporting different bombs or special operating modes can also be recalled. User/Factory Settings Menu Descriptions Reload User Default Settings: Used to restore the user setup ID settings should the program in the instrument be corrupted for any reason.
4 Menu Descriptions Calibration Data and Controls Menu Control Chart Parameters: A control chart is a graphical tool which can assist the user in determining whether or not their process is in control. Many standard methods will dictate that a reference sample be measured periodically and the results plotted on a graph. Limits for acceptable values are defined and the process is assumed to be in control as long as the results stay within these limits.
6400 Bomb 1 Menu Descriptions Manual EE Entry: This key allows the user to manually enter an EE or calibration factor for a given calorimeter ID or bomb head. If an EE value is manually entered, it is necessary to turn the Protect EE Value ON in order to prevent this value from being overwritten by an automatic update. Print Standardization Runs: This key will print all of the tests that have been incorporated into the calculated EE value.
4 Menu Descriptions Thermochemical Corrections Menu Acid Correction: Press this key on the LEFT side to toggle between Fixed HNO3, Calculated HNO3 , Entered Total, Entered HNO3, and Fixed Total for the acid correction for standardization runs. Press it on the RIGHT side to access the Acid Correction numeric dialog box on which the value can be set. An appropriate Fixed HNO3 value is 8 calories when one-gram benzoic acid pellets are used to calibrate the instrument.
6400 Calculation Factors: Accesses the Calculation Factors sub-menu, which provides for setting a number of options for the way the thermochemical corrections are applied. Calculation Factors Menu Menu Descriptions 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.
4 Menu Descriptions Net Heat/Dry Factors: Accesses the Net Heat/Dry Factors sub-menu, which provides for setting the net heat of combustion and Dry Factors Thermochemical Corrections. Data Entry Controls Menu Net Heat/Dry Heat Factors 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. Fixed Hydrogen: Press the LEFT side to toggle this setting ON/OFF.
6400 Hydrogen Entry Mode: This key steps through the options for entering hydrogen content for calculating the net heat of combustion either manually through the touch screen or automatically through the balance (USB) port. Oxygen Entry Mode: This key steps through the options for entering oxygen content for calculating the net heat of combustion either manually through the touch screen or automatically through the balance (USB) port.
4 Menu Descriptions Moisture as Determined (MAD) Entry Mode: This key steps through the options for entering the moisture as determined correction value either manually or through the touch screen or automatically through the balance (USB) port. Reporting Controls Menu Moisture as Received (MAR) Entry Mode: This key steps through the options for entering the moisture as received correction value either manually or through the touch screen or automatically through the balance (USB) port.
6400 Communication Controls Menu Menu Descriptions Customize Balance Setting. Sets the communication parameters for the balance 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. Balance Port Settings Accesses sub-menus which set the communications protocols for the printer and balances. Printer Type: Toggles between Parr 1758 and Generic.
4 Menu Descriptions »» Transfer Timeout (seconds). This value determines how long the interface will wait before giving up on a weight transfer. The value is entered in seconds. »» Balance Handler Strings. This key leads to a submenu that allows balance template to be customized for unique balances or needs. File Management Menu Log Balance to Display. Directs the incoming data stream from the balance to a display buffer.
6400 Menu Descriptions Run Data File Manager Diagnostics Menu The white upper portion of the Run Data File Manager screen presents all tests in memory in a scrollable window. Test attributes include filename (sample ID), test type, status, and date. Touching anywhere in the column related to a given test attribute will sort the file list by that attribute. Successive touches will toggle between an ascending and descending sort.
4 Menu Descriptions Data Logger 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. Data Log Destination: Options are logfile, printer or both. When the logfile option is selected, the logfile is located at /flash/log/datalog.csv.
6400 User Defined Buttons Combine Det. Reports: Pressing this key combines all determination reports into a single file named /tmp/bigdetfile.txt. Combine Std. Reports: Pressing this key combines all determination reports into a single file named /tmp/bigstdfile.txt. Logged Data to SD: Pressing this key copies the log file to an SD memory card inserted into the back of the controller. Rinse Bomb: This key initiates a bomb rinse.
5 Reports Chapter 5 Reports • Select From List. This key displays the stored results specified with the following two keys. • Run Data Type. This key enables the operator to display only determination runs, only standardization runs, only solution runs (not applicable to the 6400) or all runs. • Run Data Status. This key enables the operator to display only preliminary reports, only final reports, only pre weighed samples reports, all stored reports or preliminary and final reports.
6400 5 Notes www.parrinst.
6 Standardizations Chapter 6 Standardizations Standardizing the Calorimeter The Energy Equivalent Factor The term “standardization”, as used here, denotes the operation of the calorimeter on a standard sample from which the energy equivalent or effective heat capacity of the system can be determined. The energy equivalent, W or EE of the calorimeter is the energy required to raise the temperature one degree, usually expressed as calories per degree Celsius.
6400 Standardizations Any outliers or other tests which should not be included in the average EE Value must be deleted from the memory using the memory management procedures (see Chapter 8). A list of all tests associated with any Cal ID can be printed from the Calibration Data Page using Print Standardization Runs. The user can elect to have any number of stored standardization runs used in determining the EE value by entering this number on Calibration Data & Controls Page - Calibration Run Limit.
6 Standardizations Table 6-2 Calorimeter Control Limit Values in cal/g When Benzoic Acid is Used as a Test Sample Accepted heat of combustion taken as 6318 cal/g. Instrument precision 0.10%. Control limits based on 99% confidence (3 sigma) values. Values are in cal/g. NUMBER OF OBSERVATIONS IN A GROUP 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 50 UCL FOR THE RANGE (HIGH – LOW) WITHIN THE GROUP 23.3 27.5 29.7 31.1 32.1 32.9 33.5 34.1 34.6 35.0 35.3 35.7 36.0 36.3 36.5 36.8 37.0 37.
6400 Standardizations Table 6-3 Calorimeter Control Limit Values in BTU/lb When Benzoic Acid is Used as a Test Sample Accepted heat of combustion taken as 11373 BTU/lb. Instrument precision 0.10%. Control limits based on 99% confidence (3 sigma) values. Values are in BTU/lb. NUMBER OF OBSERVATIONS IN A GROUP 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 UCL FOR THE RANGE (HIGH – LOW) WITHIN THE GROUP 41.9 49.6 53.4 55.9 57.8 59.2 60.4 61.3 62.2 62.9 63.6 64.2 64.8 65.3 65.8 66.2 66.
7 Calculations Chapter 7 Calculations Calculating the Heat of Combustion The 6400 Calorimeter will automatically make all of the calculations necessary to produce a gross heat of combustion for the sample. However, it is important that the user understand these calculations to ensure the instrument is set up so the calculations match the procedures and the units are consistent throughout the process.
6400 Users may find it convenient to enter a fixed value for the fuse correction and avoid the need to determine this correction for each test. Fixed fuse corrections can be entered when Thermochemical Corrections, is set to ON. By default a fixed fuse correction of 50 calories is applied to all tests. Total errors of more than 3 calories will seldom occur when using a fixed fuse correction and the thread supplied by Parr.
7 Calculations Thermochemical Calculation Details Traditionally, standard solutions and procedures have been established to simplify the calculations related to the thermochemical corrections. The 6400 Calorimeter has been programmed to permit the user to use standard solutions and units which are most convenient, since the microprocessor can easily apply any conversion factors required. Acid and Sulfur Corrections • Total acid is the amount of base required to titrate the bomb washings (milliliters).
6400 Using the default acid and sulfur multipliers as well as a heat of formation of nitric acid of 14.1 cal/milliequivalent a 1 gram sample with 25 ml of washings and 2 % sulfur would result in the following calculation: e1 = [((25)(.0709)) – (2)(1)(.6238)] 14.1 e1 = [(1.7725) – (1.2476)] 14.1 e1 = [.5249] 14.1 e1 = 7.40 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.
7 Calculations ASTM Treatment for Acid and Sulfur ISO Calculations In the ASTM treatment, the correction for acid formation assumes that all the acid titrated is nitric acid. Obviously, if sulfur is present in the sample, which in turn produces sulfuric acid, part of the correction for the sulfuric acid formed is already included in the ASTM nitric acid correction (e1). This is adjusted by a separate computation based upon the sulfur content of the sample. An additional correction of 1.
6400 Calculations Spiking Samples Conversion to Other Moisture Bases It is sometimes necessary to add a spiking material to samples which are very small, have a low heat of combustion, or have a high moisture content to add sufficient heat to drive the combustion to completion. Benzoic acid is an excellent material for spiking for all of the same reasons it is a good standard material. White oil is also an excellent material, particularly for liquid samples.
8 Computer Communications Chapter 8 Computer Communications 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.
6400 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 Microsoft’s CIFS (Common Internet File System) implementation. As a result, Samba has become a de facto Microsoft network compatibility tool. In relation to CIFS, Samba allows non-Microsoft operating systems to enjoy effectively seamless server and client operation in networks catering to the needs of Windows computers.
8 Computer Communications The calorimeter offers a web server service. Test reports can be viewed with a web browser using a URL of the following form. http://10.1.5.10 Where 10.1.5.10 is the IP address of the calorimeter. The following screenshot illustrates the calorimeter home page.
6400 Computer Communications Clicking on the Config button will display the screen below. Changes made on this screen will change the settings in the calorimeter. www.parrinst.
8 Computer Communications Clicking on the Run Data button displays a list of reports currently in the instrument memory. Clicking on a test under the select sample ID box will display the data for the selected sample ID.
6400 Computer Communications Clicking on the System Info button will display the screen below. www.parrinst.
8 Computer Communications Clicking on the LCD Snap Shot button will display the current menu screen displayed by the calorimeter. If the backlight is not on, this screen will display a blank blue square. Note: This is a picture only. The calorimeter cannot be remotely operated from this screen. Remote operation requires the appropriate Feature Key. Please contact Parr Instrument Company for more details about available Feature Keys.
6400 Computer Communications Clicking on the Documentation button will display the screen below. Clicking on any of the links will open the corresponding web page. Note: Connection to the internet is required for these links. ’ www.parrinst.
8 Computer Communications 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.
6400 Computer Communications Table 8-2 6400 Calorimeter Run Data Template Field SampleID Timestamp Mode Method State Units UnitMultIfOther BombID BombEE SampleWt SpikeWt Fuse FuseFinal Acid AcidFinal Sulfur SulfurFinal Hydrogen HydrogenFinal MAD MAD Final JacketTemp InitTemp DeltaT HOC NetHOC DryHOC DryNetHOC Oxygen Description char[16] MM/DD/YY HH:mm:ss 0 = determination, 1 = standardization 0 = equilibrium, 1 = dynamic 0 = preweigh, 1 = preliminary, 2 = final 0 = MJ/kg, 1 = BTU/lb, 2 = cal/g, 3 = J/kg,
9 Memory Management Chapter 9 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 standardization 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. Clearing Memory The FILE MANAGEMENT key on the main menu leads to the file management sub-menu.
6400 9 Notes www.parrinst.
10 Maintenance Chapter 10 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 Maintenance 10 Fuses 50 to 100 Test Maintenance The replacement of protective fuses for the 6400 Calorimeter should be performed by qualified personnel. Replace the heating wire, with 2.5” 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.
10 Maintenance The 1140DD Seal/Release mechanism should be serviced with the same frequency as the bomb head. This includes the replacement and lubrication of the 659DDJU (2), 1138DD, 1143DD and 357HCJB O-rings with 811DD lubricant. See Figure 14-15 and Figure 14-16 for O-ring locations. The tools required are: screwdriver, snap ring pliers and needle nose pliers. 1. Turn off the gas supply to the calorimeter. Raise the lid. Go to the I/O Diagnostics Screen and turn on the bomb seal command.
6400 Maintenance 10 6400 Maintenance Checklist Date Quarterly Maintenance Date Date Date Date 50 to 100 Test Maintenance Date Date Date 1. Change water 2. Replace 149C 3. Clean grill on heat sink. 1. Replace 8400DD2 Heating Wire 2.
11 Troubleshooting Chapter 11 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 (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 Troubleshooting 11 The third condition can be eliminated by following the procedure outlined in the section servicing the O-rings on the 966DD2 piston and carefully inspecting the 1/8 nylon pressure hose and associated compression fittings for leaks while this circuit is maintained at operating pressure, using the calorimeter I/O diagnostics. A minute leak will result in a significant reduction in upward thrust.
11 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 selfevident and suggestions for correcting the error condition. A Postperiod Timeout has Occurred The calorimeter has failed to establish an acceptable final temperature within the time allowed.
Troubleshooting 11 6400 Bomb ID – Has Been Fired – Times Which Exceeds the Bomb Service Interval. The calorimeter controller keeps track of how many times the bomb has been fired. When this count exceeds a preset limit (usually 500) this message will be issued each time the bomb is used for a test. Perform bomb maintenance and reset counter on Calibration Data and Control page for appropriate bomb number. The heater loop break limit has been detected. The heater will now be shutdown.
12 Technical Service Chapter 12 Technical Service 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 E-mail: parr@parrinst.com Any correspondence must include the following basic information: • The model and serial # of the instrument. • Software version(s) shown on the “Software and Hardware Information” page.
Notes 12 6400 www.parrinst.
13 Parts Lists Chapter 13 Parts Lists Principal Assemblies in Calorimeter Item Description 1138/1138CL 1795E 1796E 897E A1250DD2 A1251DD A1447DD Oxygen Combustion Vessel Power Supply, 24V Power Supply, 5/12V Capacitor, Ignition Controller Assembly Oxygen Solenoid Assembly Water Solenoid Assembly A1448DD A1449DD A1254DD2EB A1254DD2EE A1255DD 1433DD A1449DD A1456DD A1275DDEB A1275DDEE 139E23 Temp Control Sub-Assy Water Chiller Assembly Pump Assembly Circulating 115V Pump Assembly Circulating 230V Propel
6400 Parts Lists A1255DD Bucket Stirrer Assembly Item 682DD 683DD 684DD Description Snap Ring, Internal .50 Wave Spring, .50 OD Ball Bearing, .
14 Drawings Chapter 14 Drawings Figure 14-1 1138 Parts Diagram 82 Parr Instrument Company
Drawings 14 6400 1138 Parts Diagram Key Key Item Description 1 888DD2 Cylinder 2 889DD Outer Ring 3 821DD O-ring 1/16 ID NBR 4 668DD Check Valve 5 882DD O-ring 1/2 ID NBR 6 925DD Bomb Retainer 7 SA1632RD06 (2) 8-32 x 3/8 RHMS 8 902DD Ground Stud Head 9 899DD Head Handle 10 1454DD Funnel 11 904DD (2) Standoff 8-32 x 5/8 M-F 12 905DD Standoff 8-32 x 3/8 M-F 13 SA1632FT06 (2) 8-32 x 3/8 FHMS 14 898DD Locator Cap 15 SN1632HX 8/32 Hex Nut 16 1374HCJV (2) O-ring
14 Drawings Figure 14-2 6400 Cutaway Right 84 Parr Instrument Company
Drawings 14 6400 Figure 14-3 6400 Cutaway Left www.parrinst.
14 Drawings Figure 14-4 6400 Cover Open 1324DD2 Locking Post 86 Parr Instrument Company
A2140E IO BOARD P6 P8 USB PORT A2154E CPU BOARD www.parrinst.com J10 J1 J9 J8 J4 1/X .... ±1/64 .00 .... ±.010 .000 .... ±.003 ANGULAR ...
14 Drawings Figure 14-6 A1251DD Oxygen Solenoid Assembly Figure 14-7 A1447DD Water Solenoid Assembly 88 Parr Instrument Company
Drawings 14 6400 Figure 14-8 A1456DD Rinse Valve Assembly www.parrinst.
14 Drawings Figure 14-9 6400 Internal Plumbing Diagram 90 Parr Instrument Company
Drawings 14 6400 Figure 14-10 6400 Water Tank and Jacket Cooling Solenoid www.parrinst.
14 Drawings Figure 14-11 A1455DD Propeller Assembly Apply thread sealant (Locktite or equivalent to set screw in 1242DD2 pulley before installing.
Drawings 14 6400 Figure 14-13 A1268DD Stirrer Motor and Mount www.parrinst.
14 Drawings Figure 14-14 6400 Bucket Assembly 94 Parr Instrument Company
Drawings 14 6400 Figure 14-15 6400 Air Can Assembly, Cutaway Left www.parrinst.
14 Drawings Figure 14-16 6400 Air Can Assembly, Cutaway Front 96 Parr Instrument Company
Drawings 14 6400 Figure 14-17 A1450DD Bomb Head Assembly, View 1 www.parrinst.
14 Drawings Figure 14-18 A1450DD Bomb Head Assembly, View 2 98 Parr Instrument Company
Drawings 14 6400 Figure 14-19 1.50 1052DD BOTTLE CAP TOLERANCES .... .... .... ±1/64 ±.010 ±.003 ANGULAR .. ±1/2° UNMARKED RADII .03" 1/X .00 .
14 Drawings Figure 14-20 Wiring Diagram 100 Parr Instrument Company
Drawings 14 6400 Figure 14-21 Wiring Diagram www.parrinst.
14 Drawings Figure 14-22 Fuse Diagram 102 Parr Instrument Company
6400 Notes www.parrinst.
15 Tables Chapter 15 Tables Table 15-1 Factory Default Settings Calorimeter Operations Operating Mode Bomb Installed/EE Heater and Pump Program Information and Controls Determination 1/940.
6400 Determination Fixed Fuse Correction Acid Correction Fixed Sulfur Correction Net Heat/Dry Factors Tables 15 Auto Sample ID Controls ON 50.0 Fixed HN03 8.0 OFF 0.
15 Tables Table 15-2 Settings for ISO & BSI Methods Page Thermochemical Corrections Line Setting Value Acid Correction (STD) Entered HNO3 13 Fixed Sulfur STD Off 7 Acid Correction (DET) Entered HNO3 13 Fixed Sulfur DET Off 7 Acid Multiplier Sulfur Value is Percent Calculations Factors Off Sulfur Multiplier Use Offset Correction Offset Value 106 0.154 Parr Instrument Company 0.1 On -43.
587M R03 02/11/14
