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6300 PREFACE — 7 Scope — 7 Explanation of Symbols — 8 Safety Information — 8 Intended Usage — 8 Cleaning & Maintenance — 8 General Specifications — 9 Environmental Conditions — 9 Getting Started — 9 CHAPTER 1 CONCEPT OF OPERATION — 11 A Highly Automated Procedure — 11 New Convenience and New Technology — 11 Isoperibol Operation — 11 Dynamic Operation — 11 Full Microprocessor Based Process Control — 12 Full Microprocessor Based Data Acquisition and Handling — 12 Flexible Programming — 12 CHAPTER 2 INSTAL
TABLE OF CONTENTS APPENDIX B CALCULATIONS — 71 Calculating the Heat of Combustion — 71 General Calculations — 71 Thermochemical Corrections — 71 Fuse Correction — 73 Acid and Sulfur Corrections — 73 ASTM Treatment for Acid and Sulfur — 74 ISO Calculations — 75 Spiking Samples — 75 Conversion to Net Heat of Combustion — 75 APPENDIX C STANDARDIZATION — 77 Standardizing the Calorimeter — 77 Standard Materials — 77 Automatic Statistical Calculations — 77 APPENDIX D COMMUNICATIONS INTERFACES — 81 USB Port —
6300 TABLE OF CONTENTS FIGURES (CONTINUED) Figure F-2 Parts Diagram for the 1138 and 1138CL Oxygen Bombs — 104 Figure F-3 6300 Oxygen Bomb Calorimeter Cutaway Right — 106 Figure F-4 6300 Oxygen Bomb Calorimeter Cutaway Left — 107 Figure F-5 6300 Oxygen Bomb Calorimeter Cover Open — 108 Figure F-6 A1250DD2 Control Schematic — 109 Figure F-7 A1251DD Oxygen Solenoid Assembly — 110 Figure F-8 A1200DD Internal Plumbing Diagram — 111 Figure F-9 A1252DD Water Solenoid Assembly — 112 Figure F-10 A1416DD Bomb Wash
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6300 PREFACE PREFACE No. 201M 207M 230M SCOPE This manual contains instructions for installing and operating the Parr 6300 Calorimeter. For ease of use, the manual is divided into nine chapters.
PREFACE EXPLANATION OF SYMBOLS I On Position O Off Position ~ Alternating Current (AC) 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.
6300 PREFACE GENERAL SPECIFICATIONS Electrical Ratings 120VAC, 6.0 Amps. 50/60 Hz 240VAC, 3.0 Amps, 50/60 Hz Before connecting the calorimeter to an electrical outlet, the user must be certain that the electrical outlet has an earth ground connection and that the line, load and other characteristics of the installation do not exceed the following limits: Voltage: Fluctuations in the line voltage should not exceed 10% of the rated nominal voltage shown on the data plate.
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6300 CHAPTER 1 CONCEPT OF OPERATION A HIGHLY AUTOMATED PROCEDURE Parr proudly introduces a new Oxygen Bomb Calorimeter, No. 6300, in which new technology is combined with time-proven calorimetric techniques to produce a completely automatic system for measuring the heat of combustion of solid and liquid fuels, combustible wastes, foods, feeds and other oxygen combustible materials.
1 CONCEPT OF OPERATION FULL MICROPROCESSOR BASED PROCESS CONTROL The microprocessor controller in this calorimeter has been pre programmed to automatically prompt the user for all required data and control input and to: • • • • • • • • • Generate all temperature readings in the calorimeter. Monitor jacket as well as bucket temperature. Confirm equilibrium conditions. Fire the bomb. Confirm that ignition has occurred. Determine and apply all necessary heat leak corrections.
6300 INSTALLATION 2 CHAPTER 2 INSTALLATION REQUIRED CONSUMABLES, UTILITIES AND POWER REQUIREMENTS INSTALLING THE CALORIMETER Each Parr 6300 Calorimeter was completely assembled and thoroughly tested prior to shipment. The following stepwise procedure will guide the user through the installation process. • Unpack the calorimeter and carefully check the individual parts against the packing list.
2 INSTALLATION INSTALLING THE CALORIMETER (CONTINUED) • Make the connections to the oxygen supply at this time. Refer to figure 2-2 and 2-3. 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.
6300 INSTALLATION 2 Fitting. Make sure that the tubing rests firmly on the shoulder of the fitting and that the nut is fingertight. 2. Before tightening the Swagelok nut, scribe the nut at the 6 o’clock position. 3. While holding the fitting body steady with a backup wrench, tighten the nut 1-1/4 turns. Watch the scribe mark, make one complete revolution and continue to the 9 o’clock position. 4. For 3/16” and 4mm or smaller tube fittings, tighten the Swagelok nut 3/4 turns from finger-tight.
2 INSTALLATION Figure 2-2 6300 Calorimeter Back Panel 16 Parr Instrument Company
6300 INSTALLATION 2 6300 CALORIMETER EXTERNAL PLUMBING Figure 2-3 Closed Loop Configuration with 6520A O2 Regulator DI Water ~Room Temp 5-10 °C Rinse Collection 6520A Water Recircualtion System Figure 2-4 Closed Loop Configuration with 1564 O2 Regulator DI Water ~Room Temp 5-10 °C 1552 Water Cooler 1564 Water Recircualtion System Rinse Collection Line 1 & 2 – Maximum length of 10 feet, 1/4” OD, Polyurethane (Part Number HJ0025TB035) Line 3 - Maximum length of 25 feet, 1/8” OD, Nylon (Part Number
2 INSTALLATION 6300 CALORIMETER EXTERNAL PLUMBING (CONTINUED) Figure 2-5 Open Loop Configuration with 1552 O2 Regulator Tap Water · <25 °C · <85 ppm · <60 psig DI Water ~Room Temp 1552 Water Cooler Rinse Collection Drain Figure 2-6 Open Loop Configuration O2 Regulator Tap Water · <25 °C · <85 ppm · <60 psig DI Water ~Room Temp 5-10 °C Rinse Collection Drain Line 1 & 2 – Maximum length of 10 feet, 1/4” OD, Polyurethane (Part Number HJ0025TB035) Line 3 - Maximum length of 25 feet, 1/8” OD, Nylon (Pa
6300 INSTALLATION 2 INSTALLING THE CALORIMETER (CONTINUED) • After the calorimeter displays the main menu, press the Calorimeter Operation button. This screen should indicate that the jacket is filling with water. The initial fill can take as long as 8 to 10 minutes to complete. If the jacket filling process times out, simply acknowledge the timeout message to resume the jacket filling process. After the jacket is filled press the Heater and Pump button in order to toggle the heater and pump on.
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6300 CHAPTER 3 INSTRUMENT DESCRIPTION TYPES OF CONTROLS All calorimeter configurations and operations are handled by a menu-driven system operated from the bright touch screen display. The settings and controls are organized into nine main sections or pages which comprise the MAIN MENU. Note: Keys with a double box in the upper left hand corner lead to sub-menus. INSTRUMENT DESCRIPTION 3 Some keys lead to multiple choices. Always clear the current value before entering a new value.
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6300 PROGRAM INSTALLATION & CONTROL 4 CHAPTER 4 PROGRAM INSTALLATION & CONTROL SOFTWARE INSTALLATION The program in the 6300 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.
4 PROGRAM INSTALLATION & CONTROL Figure 4-1 6300 Factory Default Settings Calorimeter Operations Operating Mode Bomb Installed/EE Heater and Pump Operating Controls Method of Operation Reporting Units Use Spiking Correction “OTHER” Multiplier Calibrate Touchscreen LCD Backlight Timeout(s) LCD Backlight Intensity Print Error Messages Language Spike Controls Use Spiking Heat of Combustion of Spike Use Fixed Spike Weight of Fixed Spike Prompt for Spike before Weight Bomb Rinse Tank Control Report Rinse Tank Em
6300 PROGRAM INSTALLATION & CONTROL 4 Factory Default Settings Continued Acid Multiplier Sulfur Value is Percent Sulfur Multiplier Fuse Multiplier Use Offset Correction (ISO) Offset Value Net Heat/Dry Factors Fixed Hydrogen Fixed Oxygen Fixed Nitrogen Calculate Net Heat of Combustion Fixed Moisture as Determined Fixed Moisture as Received Dry Calculation Data Entry Controls Prompt for Bomb ID Weight Entry Mode Acid Entry Mode Net Heat Entry Modes Auto Sample ID Controls Sample Weight Warning above Spike W
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6300 CHAPTER 5 OPERATING INSTRUCTIONS TO BEGIN A TEST 1. Weigh the sample to 0.1 mg. 2. Gently tap the 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.) 3. Carefully place the capsule into the capsule holder. 4. Attach 10 cm of ignition thread (see Figure 5-2). 5. Install bomb head in calorimeter. 6.
5 OPERATING INSTRUCTIONS Figure 5-1 Fill Flow Diagram 28 Parr Instrument Company
6300 ALLOWABLE SAMPLE SIZE OPERATING INSTRUCTIONS 5 Figure 5-2 Cotton Thread Assembly 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). This generally limits the mass of the combustible charge (sample plus benzoic acid, gelatin, firing oil or any combustion aid) to not more than 1.1 grams.
5 OPERATING INSTRUCTIONS WARNING - DO NOT OVERFILL THE BOMB The safety relief valve on the regulator should protect the system from an over fill. If for any reason, the bomb should accidentally be charged to more than 600 psig (40 atm), do not fire the bomb. The dangerous pressures which might develop under such conditions could damage the bomb and injure the operator.
6300 CLOSING THE BOMB Care must be taken not to disturb the sample when moving the bomb head from the support stand to the bomb cylinder in the calorimeter. Check the sealing ring to be sure that it is in good condition and moisten it with a bit of water so that it will slide freely into the cylinder. OPERATING INSTRUCTIONS 5 at the top of the bomb closes and isolates the bomb from the oxygen filling line. 3.
5 OPERATING INSTRUCTIONS Figure 5-4 Rinse & Cool Flow Diagram 32 Parr Instrument Company
6300 OPERATING INSTRUCTIONS 5 POST-PERIOD DRAIN After firing is confirmed, the post-period begins (see Figure 5-3). At the completion of the bomb rinse sequence, the drain sequence begins (see Figure 5-5). 1. The controller monitors the temperature rise and determines the final temperature rise by either the dynamic or equilibrium criteria as established by the user. 1. The water in the bucket is drained out of the bucket and routed to the drain connection. 2.
5 OPERATING INSTRUCTIONS Figure 5-5 Drain Flow Diagram 34 Parr Instrument Company
6300 SAMPLES Particle Size and Moisture Content Solid samples burn best in an oxygen bomb when reduced to 60 mesh, or smaller, and compressed into a pellet with a 2811 Parr Pellet Press. Large particles may not burn completely and small particles are easily swept out of the capsule by turbulent gases during rapid combustion. Note: Particle size is important because it influences the reaction rate.
5 OPERATING INSTRUCTIONS FOODSTUFFS AND CELLULOSIC MATERIALS Fibrous and fluffy materials generally require one of three modes of controlling the burn rate. Fibrous materials do not pelletize readily and generally require either moisture content or combustion aid such as mineral oil to retard the burn rate and avoid development of high pressures.
6300 OPERATING INSTRUCTIONS 5 Note: Tape should always be stored in a sealed container to minimize changes in its moisture and solvent content Figure 5-6 Combustion Capsule with Adhesive Tape Seal POOR COMBUSTION 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.
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6300 CORRECTIONS & FINAL REPORTS 6 CHAPTER 6 CORRECTIONS & FINAL REPORTS ENTERING CORRECTIONS AND OBTAINING THE FINAL REPORT Final reports for each test can be obtained whenever the operator is prepared to enter any required corrections for fuse, acid and sulfur. When entering corrections, the user can choose either of two methods. These are: • • Manual Entry Fixed Corrections Refer to the Reporting Instructions, Chapter 7, for the steps necessary to initiate a report from the controller.
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6300 CHAPTER 7 REPORTING INSTRUCTIONS REPORT OPTION SECTION The 6300 Calorimeter can transmit its stored test data in either of two ways. The REPORT DESTINATION key on the Reporting Controls Page toggles the report destination between the display and an optional printer connected to the USB port of the calorimeter. This page also selects the type of reports that are generated automatically by the calorimeter.
7 REPORTING INSTRUCTIONS REPORT GENERATION (CONTINUED) 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 control page is turned on.
6300 CHAPTER 8 FILE MANAGEMENT The 6300 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. FILE MANAGEMENT 8 CLEARING MEMORY The FILE MANAGEMENT key on the main menu leads to the file management sub-menu.
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6300 MAINTENANCE & TROUBLESHOOTING 9 CHAPTER 9 MAINTENANCE & TROUBLESHOOTING ROUTINE MAINTENANCE Note: See the corresponding water system manuals for information on the maintenance of those systems. To service or remove the bomb cylinder from the bucket assembly, remove the 941DD Wedge with needle nose pliers. Remove the 668DD Check Valve from the bomb cylinder. Remove the two SA1632RD18 Machine Screws (see Figure F-20). Then remove the 942DD Bushings and the 1081DD Quad-ring.
9 MAINTENANCE & TROUBLESHOOTING 500 Tests (Continued) abrasive may require this maintenance to be performed on a more frequent interval such as every 250 tests. The 882DD and 969DD O-rings should also be replaced and is positioned between the bucket and the air-can of the calorimeter. For your convenience, these parts may be purchased as kit number 6038, Firing Maintenance Kit. See Figures F-1 and F-2 for O-ring locations.
6300 MAINTENANCE & TROUBLESHOOTING 9 6300 MAINTENANCE CHECKLIST Quarterly Maintenance Date Date Date Date Date Date Date Date Change water Replace 149C Clean grill on heat sink.
9 MAINTENANCE & TROUBLESHOOTING INSPECTION OF CRITICAL SEALING SURFACES The sealing grooves and related surfaces for most of the Parr bombs are machined to tolerances as small as +/- 0.001” (0.03mm). As a result, any imperfection in a sealing surface resulting from either normal use or carelessness in handling the bomb can cause the bomb to leak. If the damage or accumulated wear is much less than 0.001” (0.03mm), then careful polishing will restore the bomb sealing to an as new condition.
6300 MAINTENANCE & TROUBLESHOOTING 9 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. This is very important and you should take proper pre-caution. 1. Make sure the 668DD check valve is installed at the bottom of the cylinder. 2. Lock the head into the cylinder and close the calorimeter lid. 3. Confirm the Exhaust is off. 4.
9 MAINTENANCE & TROUBLESHOOTING JACKET FILL AND COOLING PROBLEMS Jacket Fill Error – A problem has been detected while attempting to fill the bomb jacket; please correct the problem and press ‘OK’ to continue… Error – Could not cool the bomb successfully; check water supply and drain. Jacket Fill Error: When the water level in the jacket drops a level switch closes. This tells the CPU board (through the I/O board) that more water is needed in the jacket.
6300 MAINTENANCE & TROUBLESHOOTING 9 BOMB REMOVAL AND REPLACEMENT To service or remove the bomb cylinder from the bucket assembly, remove the 941DD Wedge with needle nose pliers. Remove the 668DD Check Valve from the bomb cylinder. Remove the two SA1631RD018 Machine Screws (see Figure F-20). Then remove the 942DD Bushings and the 1081DD Quad-ring.
9 MAINTENANCE & TROUBLESHOOTING Rinse Tank Level May Be Low. The controller decrements the rinse tank counter each time the bomb is rinsed. This message will be issued when the counter is at or below zero when the bomb rinse sequence is executed. This message is a reminder that the rinse tank needs refilling, followed by a manual resetting of the bomb rinse counter. There Is A Problem With The Bucket Thermistor. Possible electrical open. (1416E left side of bucket at bottom): • Check connection to board.
6300 MENU OPERATING INSTRUCTIONS A APPENDIX A MENU OPERATING INSTRUCTIONS The settings and controls are organized into nine main sections or pages which comprise the Main Menu. This appendix describes all pages of the menu-based operating system of the 6300 Calorimeter. 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.
A MENU OPERATING INSTRUCTIONS CALORIMETER OPERATION MENU (CONTINUED) TEMPERATURE PLOT SETUP MENU 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.
6300 MENU OPERATING INSTRUCTIONS A Jacket Plot Symbol: Toggles between: (same as Bucket Plot Color, p. 54). OPERATING CONTROLS MENU 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.
A MENU OPERATING INSTRUCTIONS OPERATING CONTROLS MENU (CONTINUED) • • 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. The heat of combustion of spike is entered on sub-menu keyboard in cal/g. • Use Fixed Spike. When set to ON, a constant amount of spike is to be added to each test. • Weight of Fixed Spike.
6300 MENU OPERATING INSTRUCTIONS A “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. It is important that a touch screen stylus, rather than a finger, be used in order to realize an accurate calibration.
A MENU OPERATING INSTRUCTIONS PROGRAM INFORMATION AND CONTROL MENU (CONTINUED) Bomb Type Select: This key toggles through the different bomb models available for the calorimeter. When the user chooses a bomb, the instrument must be re-booted to load the correct version of the software. (Note that the calorimeter will not let you exit this function without re-booting the system). User Function Setup: This key leads to sub-menus that support the configuration of five factory/user definable function keys.
6300 MENU OPERATING INSTRUCTIONS A lated by the Calorimeter and accesses the sub-menu on which this limit is set. If this value is exceeded, the user will be warned to take corrective action before proceeding with testing. A setting of zero disables this check. Heat of Combustion of Standard: Displays the heat of combustion in calories per gram for the material used to standardize the calorimeter and accesses the sub-menu on which this value is set. For benzoic acid, this value is 6318.
A MENU OPERATING INSTRUCTIONS CALIBRATION DATA AND CONTROLS MENU (CONTINUED) • Bomb Fire Count. Displays the current bomb firing count or the number of times the bomb has been fired since it was last serviced. When this count matches the limit set by Bomb Service Interval (on the Calibration Data and Controls screen), the user will be informed that the bomb is ready for service.
6300 MENU OPERATING INSTRUCTIONS A preliminary reports. When any fixed correction is set to ON, the specified value will be used in the final reports, and the 6300 will not prompt for actual corrections to be entered. (If all corrections are fixed, only a final report will be generated.) When any fixed correction is set to OFF, during the data entry reporting steps the user will be prompted to enter an appropriate desired value which will be used in the final report.
A MENU OPERATING INSTRUCTIONS THERMOCHEMICAL CALCULATIONS MENU (CONTINUED) 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. Note: When fixed corrections are turned ON, the value in the specified field will be used in both the preliminary and final reports. The calorimeter will not prompt for actual corrections.
00 MENU OPERATING INSTRUCTIONS A NET HEAT/DRY HEAT FACTORS DATA ENTRY CONTROLS MENU Fixed Hydrogen: Press the LEFT side to toggle this setting On/Off. Press the RIGHT side to display the Fixed Hydrogen numeric dialog box and change its value. 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 Oxygen: ON/OFF and value entry. Fixed Nitrogen: ON/OFF and value entry. Calculate Net Heat of Combustion: ON/OFF.
A MENU OPERATING INSTRUCTIONS DATA ENTRY CONTROLS MENU (CONTINUED) 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.
6300 MENU OPERATING INSTRUCTIONS A Moisture as Received 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. Auto Preweigh ID Controls: Accesses sub-menu, used to automatically assign Sample ID numbers when a series of samples are pre weighed ahead of the time they are actually tested. • Automatic Preweigh ID. ON/OFF toggle for this feature.
A MENU OPERATING INSTRUCTIONS REPORTING CONTROLS MENU (CONTINUED) Balance Port: Accesses sub-menu, Balance Port Communications. Use New EE Value in Recalculation: When set to ON, any recalculation made will use the most recent EE value in the calculations. In the OFF position, all calculations will be made using the EE value which was effective when the test was originally run. Report Schedule: Toggles between End of Post Period and end of Cool/ Rinse.
6300 MENU OPERATING INSTRUCTIONS A FILE MANAGEMENT » » » • • 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. 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.
A MENU OPERATING INSTRUCTIONS 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.
6300 MENU OPERATING INSTRUCTIONS A 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. Helpful items to log are: » D0 - Corrected calorimeter drift rate » Tsum - Accumulated temperature rise » T1 - Extrapolated temperature rise » C0 - Temperature conversion counter • Data Logger. This key toggles the data logging function ON/OFF. • Data Log Interval.
A MENU OPERATING INSTRUCTIONS DIAGNOSTICS MENU (CONTINUED) • 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. I/O Diagnostics: Rinse Bomb: This key initiates a bomb rinse. This function can be used to clean out the cylinder in the event a sample is spilled inside the cylinder.
6300 CALCULATIONS B APPENDIX B CALCULATIONS CALCULATING THE HEAT OF COMBUSTION The 6300 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.
B CALCULATIONS THERMOCHEMICAL CORRECTIONS (CONTINUED) the user prefers. Care must be used to ensure the proper corrections are applied, and the calculations made are consistent with the procedure used. be calculated. In the 6300 Calorimeter this is a fixed correction of 10 calories per test. Users may find it convenient to enter a fixed value for the acid correction and avoid the need to determine this correction for each test. Use of a fixed value for the acid correction is highly recommended.
6300 the thermochemical corrections. The 6300 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.
B CALCULATIONS ACID AND SULFUR CORRECTIONS (CONTINUED) Example: For a test run with energy equivalent of 927.4022 and a corrected temperature rise of 6.892 would result: Fixed Total: The Acid Correction represents the total base required to titrate the bomb washings (in milliliters). This includes both nitric and sulfuric acid. The correction is a fixed value set by the operator. e1 = (1.58/1000)(927.4022)(6.892) e1 = 10.
6300 ISO CALCULATIONS Both the ISO 1928 and BSI 1016: Part 5 methods for testing the calorific value of coal and coke, deal with acid and sulfur corrections in a manner which is somewhat different than ASTM procedures. Provision has been made in the 6300 Controller for dealing with these different procedures. The analysis of bomb washings in these methods call for a titration, first using 0.1N barium hydroxide (V2) followed by filtering, and a second titration using 0.1N HCL(V1) after 20 mL of a 0.
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6300 STANDARDIZATION C APPENDIX C STANDARDIZATION 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.
C STANDARDIZATION AUTOMATIC STATISTICAL CALCULATIONS (CONTINUED) 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. 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).
6300 STANDARDIZATION C Table C-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 UCL FOR THE RANGE OBSERVATIONS (HIGH – LOW) IN A GROUP WITHIN THE GROUP 1 2 23.3 3 27.5 4 29.7 5 31.1 6 32.1 7 32.9 8 33.5 9 34.1 10 34.6 11 35.0 12 35.3 13 35.7 14 36.0 15 36.3 16 36.5 17 36.8 18 37.0 19 37.2 20 37.4 21 37.
C STANDARDIZATION Table C-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 UCL FOR THE RANGE OBSERVATIONS (HIGH – LOW) IN A GROUP WITHIN THE GROUP 1 2 41.9 3 49.6 4 53.4 5 55.9 6 57.8 7 59.2 8 60.4 9 61.3 10 62.2 11 62.9 12 63.6 13 64.2 14 64.8 15 65.3 16 65.8 17 66.2 18 66.6 19 67.0 20 67.4 21 67.
6300 COMMUNICATIONS INTERFACES D APPENDIX D METTLER 011/012 BALANCE INTERFACE COMMUNICATIONS INTERFACES Field ID space data space g CR LF USB PORT USB Connection The 6300 Calorimeter is equipped with a USB port for connection to either a 40 or 80 column printer and/or a computer. The default parameters for the 6300 Calorimeter are set up for use with the Parr 1758 Printer. BALANCE AND PORT INPUT DRIVER SPECIFICATIONS The 6300 Calorimeter supports input from multiple balance types.
D COMMUNICATIONS INTERFACES GENERIC INTERFACE Field data CR Length 9 1 The data field should consist of 9 numeric characters (0 through 9, +, - and space) terminated with a carriage return (CR). Leading zeros may be blanked as spaces and are counted. Non-numeric characters are ignored and will reset the input buffer if the data field has not been filled. Any characters received after filling the data field and before the carriage return are ignored.
6300 ETHERNET INTERFACE Calorimeter 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 or a static IP address can be assigned. The address can be seen on the “software and hardware info” page, under “program information and control”.
D COMMUNICATIONS INTERFACES SAMBA SERVER FEATURE (OPTIONAL) Samba was originally developed as an implementation of the SMB (Server Message Block) protocol. The most common use of SMB is in Mircosoft’s CIFS (Common Internet File System) implementation. As a result, Samba has become a de facto Microsoft network compatibility tool. In relation to CIFS, Samba allows nonMicrosoft operating systems to enjoy effectively seamless server and client operation in networks catering to the needs of Windows computers.
6300 COMMUNICATIONS INTERFACES D The following screenshot illustrates the contents of the calorimeter data directory as presented by a web browser. www.parrinst.
D COMMUNICATIONS INTERFACES 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.
6300 COMMUNICATIONS INTERFACES D Clicking on the Config button will display the screen below. Changes made on this screen will change the settings in the calorimeter. www.parrinst.
D COMMUNICATIONS INTERFACES 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.
6300 COMMUNICATIONS INTERFACES D Clicking on the System Info button will display the screen below. www.parrinst.
D COMMUNICATIONS INTERFACES 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.
6300 COMMUNICATIONS INTERFACES D 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.
D COMMUNICATIONS INTERFACES BAR CODE PORT NETWORK DATA SERVICES 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. These keys allow the user to specify the IP addresses of one or more Balance Interface devices on the network.
6300 APPENDIX E 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: 800-872-7720 Fax: (309) 762-9453 E-mail: parr@parrinst.com Any correspondence must include the following basic information: 1. The model and serial # of the instrument. 2. Software version(s) shown on the “Software and Hardware Information” page.
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6300 PARTS LISTS & DRAWINGS APPENDIX F PARTS LISTS & DRAWINGS PRINCIPAL ASSEMBLIES IN CALORIMETER Item 1136/1136CL 1138/1138CL 1795E 1796E 379VB2 412VB 533VBAD 897E 909E 911E A1050DD A1250DD2 A1251DD A1252DD A1416DD A1254DDEB A1254DDEE A1255DD A1256DD A1257DD A1260DD A1264DD A1265DD A1275DDEB A1275DDEE A1274DD 139E23 1641E 1641E2 997E5 Description O2 Combustion Vessel, 340 mL O2 Combustion Vessel, 250 mL Power Supply, 24V Power Supply, 5/12V Barbed Tee, 3/8T X 1/2T X 3/8T Union Fitting, drain Union Reduce
F PARTS LISTS & DRAWINGS A1250DD2 CONTROLLER ASSEMBLY Item 1926E A1821E A1822E A1823E A2140E A2141E A2154E A2163E A2164E A2166E A2167E 1477DD 2147E 1472DD Description Film Guard, LCD 1802E Speaker Assembly with Cable Power Cable Assembly Touchscreen Cable Assembly, 12” I/O Board LCD Transition Board CPU Board (GCM) LCD Cable Backlight Control Cable I/O to CPU USB Cable USB Peripheral Cable Display Kyrocera/Hantronix Gasket LCD LCD Encasement - Kyrocera A1251DD OXYGEN SOLENOID ASSEMBLY Item 180VB 243VB2 52
6300 PARTS LISTS & DRAWINGS A1257DD WATER REGULATOR ASSEMBLY Item 1211DD 1244DD 1245DD 447VB 60HW3HJ Description Bracket, Water Regulator Regulator, Water, 6300 Filter, Water, 1/4 NPT Connector, Female, 1/4 T X 1/4 NPTF Hose Barb, Nylon A1258DD TEMPERATURE CONTROL ASSEMBLY Item 1249DD 1417E 538VB 248HWHJ 386VB 413VB 405VB A1275DDEB A1275DDEE Description Manifold, Temperature Control Thermistor, Jacket Connector, Male, 1/8 NPTM-T-BT Nylon Elbow, Hose Barb, 1/2 T x 1/2 M, Nylon Nipple, 1/2 NPT Nylon Cap,
F PARTS LISTS & DRAWINGS A1264DD AIR CAN ASSEMBLY Item 328E 344VB 357HCJB 659DD 857DD 882DD 941DD 942DD 962DD 963DD 964DD 965DD 966DD2 967DD 969DD 970DD 1037DD 1137DD 1138DD 1139DD 1140DD 1141DD 1143DD 1235DD A1248DD2 A92HWAD 1224DD2 1226DD 98 Parr Description Hole Plug, 3/8” Connector, Male 1/8T x 1/16NPTM O-ring, Buna-N, 1/4 ID O-ring, Buna-N .5/32” ID x 1/16 C ID O-ring, Buna-N 3/8 ID O-ring, Buna-N .
6300 PARTS LISTS & DRAWINGS A1267DD ACCESSORY/INSTALLATION KIT Item 231C2 271C 3415 356HCW 43AS 811DD 840DD2 845DD2 876DD 1005DD 1347DD A1006DD A1336DD A38A A1271DD TX03SK TX09SK TX12SK TX06SK TX14SK 149C 1344DD 1889E HJ0025TB035 JT0038TB062A Description Container, PP 10L Foldable Cap w/ 7/16 Hole for Container Benzoic Acid Pellets 100 Gram Bottle O-ring, Pliers for Snap Ring Capsule, SS Lube/Sealant Heating Wire Ignition Thread, 4” Cutter, Plastic Tubing Forceps Elbow Waste Tube Assembly Drain Tube Assem
F PARTS LISTS & DRAWINGS 6300 STIRRER MOTOR AND DRIVE A1255DD BUCKET STIRRER ASSEMBLY Item 682DD 683DD 684DD 690DD 715HC 954DD 1029DD 1242DD2 SA114ORD04 SN1140HLHJ Description Snap Ring, Internal .50 Wave Spring, .50 OD Ball Bearing, .
6300 PARTS LISTS & DRAWINGS 6309B SPARE PARTS KIT Item 643DD 906DD 668DD 845DD2 3415 43AS 944DD 857DD 1094DD 1095DD 6038 359VB 1235DD 1241DD A1395DD 1245DD Description Pin, Check Valve Capsule Holder (1136) Check Valve Ignition Thread, 4” 10g ~1000 Benzoic Acid, 1.
F PARTS LISTS & DRAWINGS Figure F-1 Parts Diagram for the 1136 and 1136CL Oxygen Bombs 102 Parr Instrument Company
6300 PARTS LISTS & DRAWINGS 1136 AND 1136CL OXYGEN BOMB Key No.
F PARTS LISTS & DRAWINGS Figure F-2 Parts Diagram for the 1138 and 1138CL Oxygen Bombs 104 Parr Instrument Company
6300 PARTS LISTS & DRAWINGS 1138 AND 1138CL OXYGEN BOMB Key No.
F PARTS LISTS & DRAWINGS Figure F-3 6300 Oxygen Bomb Calorimeter Cutaway Right 106 Parr Instrument Company
6300 PARTS LISTS & DRAWINGS Figure F-4 6300 Oxygen Bomb Calorimeter Cutaway Left www.parrinst.
F PARTS LISTS & DRAWINGS Figure F-5 6300 Oxygen Bomb Calorimeter Cover Open 108 Parr Instrument Company
A2140E IO BOARD P6 P8 USB PORT www.parrinst.com J10 J1 J9 J8 J4 J100 J19 J17 J6 J5 2147E LCD DISPLAY CONNECTS IN UPPER PORT OF J4 OF CPU A2167E USB PERIPHERAL CABLE ASSY A2163E LCD CABLE ASSY A1823E TOUCH SCREEN CABLE ASSY A1821E SPEAKER CABLE ASSEMBLY A2164E BACKLIGHT CONTROL CABLE ASSY Electrostatic Discharge (ESD) hazards. Observe precautions for handling electrostatic sensitive devices.
F PARTS LISTS & DRAWINGS Figure F-7 A1251DD Oxygen Solenoid Assembly 110 Parr Instrument Company
6300 PARTS LISTS & DRAWINGS Figure F-8 A1200DD Internal Plumbing Diagram www.parrinst.
F PARTS LISTS & DRAWINGS Figure F-9 A1252DD Water Solenoid Assembly 112 Parr Instrument Company
6300 PARTS LISTS & DRAWINGS Figure F-10 A1416DD Bomb Wash Pump Assembly and Fittings www.parrinst.
F PARTS LISTS & DRAWINGS Figure F-11 A1254DD Circulatory Pump Assembly 114 Parr Instrument Company
6300 PARTS LISTS & DRAWINGS Figure F-12 A1255DD Bucket Stirrer Assembly Note: Apply thread sealant (Locktite or equivalent) to set screw in 1242DD2 pulley before installing. www.parrinst.
F PARTS LISTS & DRAWINGS Figure F-13 A1256DD Water Assembly Tank 116 Parr Instrument Company
6300 PARTS LISTS & DRAWINGS Figure F-14 A1257DD Water Regulator Assembly www.parrinst.
F PARTS LISTS & DRAWINGS Figure F-15 A1258DD Temperature Control Assembly 118 Parr Instrument Company
6300 PARTS LISTS & DRAWINGS Figure F-16 Cover Contact Pin Assembly www.parrinst.
F PARTS LISTS & DRAWINGS Figure F-17 Stirrer Motor and Mount 120 Parr Instrument Company
6300 PARTS LISTS & DRAWINGS Figure F-18 A1260DD Water Level Control Assembly www.parrinst.
F PARTS LISTS & DRAWINGS Figure F-19 A1265DD Bucket Assembly 122 Parr Instrument Company
6300 PARTS LISTS & DRAWINGS Figure F-20 6300 Air Can Assembly www.parrinst.
F PARTS LISTS & DRAWINGS Figure F-21 A1450DD Bomb Head Assembly (1) 124 Parr Instrument Company
6300 PARTS LISTS & DRAWINGS Figure F-22 A1450DD Bomb Head Assembly (2) www.parrinst.
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6300 BOMB RINSE CONTAINER ASSEMBLY G APPENDIX G BOMB RINSE CONTAINER ASSEMBLY OVERVIEW The A1050DD Bomb Rinse Container Assembly is provided as an accessory to the 6300 Calorimeter. This device allows for complete and systematic recovery of the bomb combustion products. These combustion products include that portion which is released during the initial bomb exhaust, followed by the portion expelled during the bomb rinse cycle.
G BOMB RINSE CONTAINER ASSEMBLY OPERATION (CONTINUED) Samples to be analyzed for chlorine should be spiked in a manner to insure that the sample as-burned contains less than 10% chlorine and liberates at least 5000 calories. Five thousand calories corresponds to roughly a 6.4 °C temperature rise in a 6300 Calorimeter. At the completion of the test, the collection bottle should be unscrewed from the 1052DD Bottle Cap and the contents of the combustion capsule added to the collected washings.
Parr Instrument Company 211 53rd Street Moline, Illinois 61265 USA Phone: 1-309-762-7716 or 1-800-872-7720 Fax: 1-309-762-9453 E-mail: parr@parrinst.com http://www.parrinst.
