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7

Calculations

P a r r   I n s t r u m e n t   C o m p a n y

52

c

haPter

 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 impor-
tant 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. 
 

General Calculations

The calculation for the gross heat of combustion is 
done by: 

H

c

 =

WT-e

1

 - e

2

 - e

3

m

Where:
H

c

= Gross heat of combustion.

T

= Observed temperature rise.

W

= Energy equivalent of the 

calorimeter being used.

e1

= Heat produced by burning 

the nitrogen portion of the air 
trapped in the bomb to form 
nitric acid. 

e2

= The heat produced by the 

formation of sulfuric acid from 
the reaction of sulfur dioxide, 
water and oxygen.

e3

= Heat produced by the heating 

wire and cotton thread.

m

= Mass of the sample.

 

These calculations are made in cal/g and degrees 

Celsius and then converted to other units if required.

Temperature Rise

The 6400 Calorimeter produces a corrected tempera-
ture rise reading automatically. Corrections for heat 
leaks during the test are applied. For a complete 
discussion of this process see Introduction to Bomb 
Calorimetry, Manual No. 483M.

Energy Equivalent

The energy equivalent (represented by W in the 
formula, or abbreviated as EE) is determined by 
standardizing the calorimeter as described in Chap-
ter 6 - Standardization. It is an expression of the 
amount of energy required to raise the temperature 
of the calorimeter one degree. It is commonly 
expressed in calories per degree Celsius. Since it 
is directly related to the mass of the calorimeter, 
it will change whenever any of the components of 
the calorimeter (i.e. the bomb, bucket or amount of 
water) is changed.

Thermochemical Corrections

 

Nitric Acid Correction

In the high pressure oxygen environment within the 
oxygen bomb, nitrogen that was present as part of 
the air trapped in the bomb is burned to nitric oxide 
which combines with water vapor to form nitric 
acid. All of this heat is artificial since it is not a result 
of the sample burning. The nitric acid correction 
removes this excess heat from the calculation.

Sulfur Correction

In the oxygen rich atmosphere within the bomb, 
sulfur in the sample is oxidized to sulfur trioxide 
which combines with water vapor to form sulfuric 
acid. This liberates additional heat over the normal 
combustion process which converts sulfur to sulfur 
dioxide. The sulfur correction removes this excess 
heat from the calculation.
 

Fuse Correction

The fuse correction applied by the calorimeter is 
calculated as:

e3

= (fuse value) (fuse multiplier from 

calculation factors page)

 “Fuse Value” is the number entered by the user and 
the value which appears in the test report.

Note:

  Calculation Factors - Fuse Multiplier is 

normally set to 1.0 so the entered value is in 

calories.

Summary of Contents for 6400

Page 1: ...587M 6400 Automatic Isoperibol Calorimeter Operating Instruction Manual For models produced after October 2010...

Page 2: ......

Page 3: ...ocess 22 Closing the bomb 22 Cool Rinse 26 Drain Fill Cycle 23 Pre Period 24 Bomb Firing 25 Post Period 25 Chapter 4 28 Menu Descriptions 28 Main Menu 28 Calorimeter Operation Menu 28 Temperature vs T...

Page 4: ...Server Feature Optional 59 Bar Code Port 66 Chapter 9 68 Memory Management 68 Clearing Memory 68 Removable SD Memory 68 Chapter 10 70 Maintenance 70 Inspection of Critical Sealing Surfaces 70 Bomb Re...

Page 5: ...gure 14 10 6400 Water Tank and Jacket Cooling Solenoid 91 Tables Table 6 1 Calorimeter Control Limit Values in J g When Benzoic Acid is Used as a Test Sample 49 Table 6 2 Calorimeter Control Limit Val...

Page 6: ...his book No Description 201M Limited Warranty 207M Analytical Methods for Oxygen Bombs 230M Safety in the Operation of Laboratory and Pressure Vessels 483M Introduction to Bomb Calorimetry Note The un...

Page 7: ...t specified by Parr Instrument Company the protection pro vided by the equipment may be impaired Explanation of Symbols I On Position O Off Position Alternating Current This CAUTION symbol may be pres...

Page 8: ...ditions Operating 15 C to 30 C maximum relative humid ity of 80 non condensing Installation Category II over voltage in accordance with IEC 664 Pollution degree 2 in accordance with IEC 664 Altitude L...

Page 9: ...w w w p a r r i n s t c o m 7 Notes 6400...

Page 10: ...rain SwagelokTube Fittings When SwagelokTube Fittings are used the instruc tions for installation are 1 Simply insert the tubing into the SwagelokTube Fitting Make sure that the tubing rests firmly on...

Page 11: ...r are required to fill the external pressurized rinse tank Approximately 2L of distilled de ionized or tap water with a total hardness of 85 ppm or less are required for filling the internal cooling r...

Page 12: ...1 Installation P a r r I n s t r u m e n t C o m p a n y 10 Figure 1 2 6400 Calorimeter Back Panel...

Page 13: ...l initially accept about 2 liters Fill the external rinse tank with about 16 liters of distilled water through the large opening at the top Figure 1 3 6400 External Plumbing 06 05 07 HJA of the tank T...

Page 14: ...en filling system Keep all threads fit tings and gaskets clean and in good condition Note To release the pressure inside the rinse tank turn off the gas supply and open the gas relief valve lever Gas...

Page 15: ...the Network Data Device menu in the Communications Controls menu Balance Interface devices are polled from device 1 to 15 for sample and or spike weights when the weight entry mode is set to Network...

Page 16: ...1 Installation P a r r I n s t r u m e n t C o m p a n y 14 Figure 1 4 6400 Calorimeter Peripherals Figure 1 5 Multiple Alternate Configurations...

Page 17: ...w w w p a r r i n s t c o m 15 Notes 6400 1...

Page 18: ...head in the calorimeter 6 Close the calorimeter cover making sure that the latch is engaged 7 Select determination or standardization as ap propriate on the Calorimeter Operation page by toggling the...

Page 19: ...w w w p a r r i n s t c o m 17 Notes 6400 2...

Page 20: ...nd the new value will be displayed in the lower right corner of the key 4 Data Displays Most of these keys display values that have been calculated by the calorimeter and are informational only Certai...

Page 21: ...etting go to the Pro gram Info and Control Page User Factory Settings Re load User Default Settings andYES Sample Preparation Sample Size To stay within safe limits the bomb should never be charged wi...

Page 22: ...us and fluffy materials generally require one of three modes for controlling the burn rate Fibrous materials do not pelletize readily and generally require either moisture content or a combustion aid...

Page 23: ...lowing procedure when filling and han dling any of these tape sealed sample holders 1 Weigh the empty cup or capsule then cover the top with tape trim with a knife and press the trimmed edge firmly ag...

Page 24: ...or 43A3KQ Fused Quartz 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...

Page 25: ...ty 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...

Page 26: ...e 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...

Page 27: ...period A warning of short beeps is sounded indicating the bomb is about to be fired Post Period A minimal temperature rise will confirm that the sample has ignited After this verification the post per...

Page 28: ...ed and the residual pressure is released through the bomb ex haust line 3 Once the excess oxygen is vented the bomb rinse water from the rinse water tank is admitted through the bomb rinse solenoid va...

Page 29: ...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...

Page 30: ...st or pretest in progress Calorimeter Operation Menu The Calorimeter will normally be operated from the Calorimeter Operation Menu although tests can always be started from any menu screen Operating M...

Page 31: ...minimum bucket value Jacket Plot Symbol Toggles between 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...

Page 32: ...on Spiking Controls Use Spiking When set to ON the calorimeter will prompt for the weight of the spike added and will compensate for the heat of combus tion in the calculations Heat of Combustion of S...

Page 33: ...begins The factory default value is 2s ClearTime 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 rin...

Page 34: ...ens a window with a slide adjustment to set the volume of the key cliks and alarms of the calorimeter Default is 85 Software and Hardware Info This screen displays important information such as the ma...

Page 35: ...y once the user has config ured the instrument to their operating require ments Compare Settings With Factory Defaults This button will bring up a screen that will show the differences in the current...

Page 36: ...ntrol chart is a graphical tool which can assist the user in deter mining whether or not their process is in control Many standard methods will dictate that a reference sample be measured periodically...

Page 37: ...the Calibration Data and Controls menu If the Protect EE value is set to ON this key is not functional Manual EE Entry This key allows the user to manually enter an EE or calibration factor for a give...

Page 38: ...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 Fixed Sulfur Correction Press this key o...

Page 39: ...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 Fuse...

Page 40: ...nd set the value Units are weight Fixed Moisture as Received Press the LEFT side to toggle ON or OFF whether to use the entered moisture correction Press the RIGHT side to access the Fixed Moisture as...

Page 41: ...fix for all sample IDs if the Auto matic Sample ID is set to ON Press this key to access a sub menu for entering an alphanu meric prefix Next Auto Sample ID Number Establishes the initial sample numbe...

Page 42: ...idth of the printer to either 40 or 80 columns Select 40 when the 1758 Printer is used Automatic Reporting Toggles the automatic report ing ON OFF When ON preliminary reports will be generated at the...

Page 43: ...d rate and balance type are provided to match any devices that might be connected to these ports Balance Port Settings Number of Data Bits Standard options for data bits Toggles between 7 and 8 Parity...

Page 44: ...Accesses a submenu to set up a Bar Code Scanner for use with the calorimeter Network Data Devices Accesses a submenu to input the IP addresses of networked devices such as balances and proximate analy...

Page 45: ...in blue Desel All This key deselects all files previously selected Rename This key allows the user to rename the blue highlighted filename Delete This key deletes all selected files ConvertType This k...

Page 46: ...ll 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 D...

Page 47: ...is key to display a screen with current operating system information statistics such as Processes and their associated PIDs Memory Mass Storage Network Press the Print key to print this information Vi...

Page 48: ...ly pre weighed samples reports all stored reports or preliminary and final reports Prompt For FinalValues When turned on the controller will prompt the operator to enter any missing corrections for fu...

Page 49: ...w w w p a r r i n s t c o m 47 Notes 6400 5...

Page 50: ...ellets Part No 3415 is furnished with each calorimeter for standardizing purposes The Parr benzoic acid has been calibrated against NIST benzoic acid Addition al benzoic acid pellets can be obtained f...

Page 51: ...ter a value appropriate for the test being made Table 6 1 Calorimeter Control Limit Values in J g When Benzoic Acid is Used as aTest Sample Accepted heat of combustion taken as 26454 J g Instrument pr...

Page 52: ...WITHIN THE GROUP UCL FORTHE RSD WITHIN THE GROUP MAXIMUM PERMISSIBLE DEVIATION OFTHE GROUP MEAN FROMTHE ACCEPTED VALUE OR GRAND MEAN 1 19 0 2 23 3 0 261 13 4 3 27 5 0 228 10 9 4 29 7 0 209 9 5 5 31 1...

Page 53: ...THE GROUP UCL FORTHE RSD WITHIN THE GROUP MAXIMUM PERMISSIBLE DEVIATION OFTHE GROUP MEAN FROMTHE ACCEPTED VALUE OR GRAND MEAN 1 34 1 2 41 9 0 261 24 1 3 49 6 0 228 19 7 4 53 4 0 209 17 1 5 55 9 0 196...

Page 54: ...in the formula or abbreviated as EE is determined by standardizing the calorimeter as described in Chap ter 6 Standardization It is an expression of the amount of energy required to raise the tempera...

Page 55: ...before it ignites Using the fine thread mentioned above the fuse correction for the calorimeter would be the 10 calories from electrical heating plus 12 calories from the burning thread for a total of...

Page 56: ...mple 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...

Page 57: ...plied to samples containing up to 2 nitrogen without introducing a significant error in the resulting heat of combustion value Users may find it convenient to enter a fixed value for the acid correcti...

Page 58: ...lculations 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 proced...

Page 59: ...bove 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 we...

Page 60: ...nected to LAN side of the router The PC in turn is also connected to the LAN side of the router using a similar CAT 5 cable A D Link 614 router is recommended for this purpose For this router operated...

Page 61: ...eature can be used to facilitate data file transfer from a calorimeter or proximate interface to a PC running the Windows operating system This method of file transfer for some users may be less cumbe...

Page 62: ...n y 60 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...

Page 63: ...ComputerCommunications 6400 8 w w w p a r r i n s t c o m 61 Clicking on the Config button will display the screen below Changes made on this screen will change the settings in the calorimeter...

Page 64: ...r I n s t r u m e n t C o m p a n y 62 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...

Page 65: ...ComputerCommunications 6400 8 w w w p a r r i n s t c o m 63 Clicking on the System Info button will display the screen below...

Page 66: ...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 Re...

Page 67: ...8 w w w p a r r i n s t c o m 65 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 i...

Page 68: ...eature Key and enter the feature key purchased from Parr Instrument Company into the instrument by using the touchpad Pressing the key labeled ABC allows the user to switch from upper case letters to...

Page 69: ...Hydrogen hydrogen value net calc option HydrogenFinal hydrogen value is final net calc option MAD moisture as determined value dry calc option MAD Final moisture as determined is final JacketTemp jack...

Page 70: ...troller will then ask the user to confirm that this file is to be deleted A series of files can be deleted by selecting the first file in the series and then the last file in the series using the EXTE...

Page 71: ...w w w p a r r i n s t c o m 69 Notes 6400 9...

Page 72: ...bombs with significant imper fection of this nature be serviced at Parr CAUTION Do not pry elastomer seals O rings and quad rings from seal grooves with metallic tools The use of dental picks and othe...

Page 73: ...ter Clean the grill on the heat sink at the rear of the calorimeter Periodic cleaning may be performed on the exterior surfaces of the instrument with a damp cloth All power should be disconnected whe...

Page 74: ...s oriented toward the left side of the instrument The insert is keyed to the cylinder and can not be fully inserted unless it is properly oriented 5000Test Maintenance To deal with the realities of to...

Page 75: ...Date Date Date Date 1 Replace 8400DD2 Heating Wire 2 Clean 986DD Electrode Contact Pins 500Test Maintenance Replace the following Date Date Date Date Head 1374HCJV 2 O rings 394HC O ring 694DD O ring...

Page 76: ...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 precaution 1 Make sure the 668DD check valve i...

Page 77: ...cated For reference purposes the normal upward thrust generated by the 966DD2 piston is 50 pounds The downward thrust is 20 pounds Far less than 20 pounds are required to move the piston in either dir...

Page 78: ...he bomb within the time allowed Possible causes for this error are listed below A bomb leak Poor bucket stirring Lid not tight A Postperiod Timeout has Occurred The calorimeter has failed to establish...

Page 79: ...detected The heater will now be shutdown This error means that the calorimeter is trying to heat the water in the unit for an extended period of time When the heater and pump are initially turned on t...

Page 80: ...e it is helpful if the person is close to the instrument in order to implement any changes recommended by theTechnical Service Department Return for Repair To return the instrument for repair please c...

Page 81: ...w w w p a r r i n s t c o m 79 Notes 6400 12...

Page 82: ...e Heater Assembly 230V 139E23 Fuse Fast Act 15 AMP 250V Caution For continued protection against possible hazard replace fuses with same type and rating of fuse A1250DD2 Controller Assembly Item Descr...

Page 83: ...ing 0 125 ID SN1332HX 6 32 Hex Nut 18 8 SS A1400DD Plunger Knob Assembly 1218DD Cover Air 1229DD3 Plate 1237DD2 Friction Hinge 1396DD Latch Block 1324DD2 Post Latch Locking A1230DD2 Cover Tubing Assem...

Page 84: ...14 Drawings P a r r I n s t r u m e n t C o m p a n y 82 Chapter 14 Drawings Figure 14 1 1138 Parts Diagram...

Page 85: ...DDJB O ring 1 5 8 ID NBR 21 1452DD Head 1452DDCL Head for Chlorine Service 22 655DD 2 Electrode Spacer 23 1095DD Electrode 24 PA1332RD04 2 6 32 x 1 4 RHMS 25 656DD Reducer Bushing 26 653DD Electrode N...

Page 86: ...14 Drawings P a r r I n s t r u m e n t C o m p a n y 84 Figure 14 2 6400 Cutaway Right...

Page 87: ...Drawings 6400 14 w w w p a r r i n s t c o m 85 Figure 14 3 6400 Cutaway Left...

Page 88: ...14 Drawings P a r r I n s t r u m e n t C o m p a n y 86 Figure 14 4 6400 Cover Open 1324DD2 Locking Post...

Page 89: ...F CPU A1822E POWER CABLE ASSY A2166E IO TO CPU USB CABLE ASSY RED WIRE ON CABLE CONNECTS TO PIN 1 A2154E CPU BOARD A2165E REF A BY BY SCALE DWG NO DATE DRAWN DESCRIPTION REVISIONS FOR DATE CONTROLLER...

Page 90: ...14 Drawings P a r r I n s t r u m e n t C o m p a n y 88 Figure 14 6 A1251DD Oxygen Solenoid Assembly Figure 14 7 A1447DD Water Solenoid Assembly...

Page 91: ...Drawings 6400 14 w w w p a r r i n s t c o m 89 Figure 14 8 A1456DD Rinse Valve Assembly...

Page 92: ...14 Drawings P a r r I n s t r u m e n t C o m p a n y 90 Figure 14 9 6400 Internal Plumbing Diagram...

Page 93: ...Drawings 6400 14 w w w p a r r i n s t c o m 91 Figure 14 10 6400 Water Tank and Jacket Cooling Solenoid...

Page 94: ...I n s t r u m e n t C o m p a n y 92 Figure 14 11 A1455DD Propeller Assembly Apply thread sealant Locktite or equivalent to set screw in 1242DD2 pulley before installing Figure 14 12 A1448DD Temperatu...

Page 95: ...Drawings 6400 14 w w w p a r r i n s t c o m 93 Figure 14 13 A1268DD Stirrer Motor and Mount...

Page 96: ...14 Drawings P a r r I n s t r u m e n t C o m p a n y 94 Figure 14 14 6400 Bucket Assembly...

Page 97: ...Drawings 6400 14 w w w p a r r i n s t c o m 95 Figure 14 15 6400 Air Can Assembly Cutaway Left...

Page 98: ...14 Drawings P a r r I n s t r u m e n t C o m p a n y 96 Figure 14 16 6400 Air Can Assembly Cutaway Front...

Page 99: ...Drawings 6400 14 w w w p a r r i n s t c o m 97 Figure 14 17 A1450DD Bomb Head Assembly View 1...

Page 100: ...14 Drawings P a r r I n s t r u m e n t C o m p a n y 98 Figure 14 18 A1450DD Bomb Head Assembly View 2...

Page 101: ...051DD EXHAUST DIFFUSER 308VBAD MALE CONNECTOR 1 4T 1 4NPTM HX0025TB062 1 4 TUBING X 4 FT LG 411VBAD REDUCER 1 4T 3 8Tx 221VBAD 3 8T NUT 222VBAD 3 8T FERRULE SET SEE NOTE 1 NOTES 1 CONNECTS TO VESSEL E...

Page 102: ...14 Drawings P a r r I n s t r u m e n t C o m p a n y 100 Figure 14 20 Wiring Diagram...

Page 103: ...Drawings 6400 14 w w w p a r r i n s t c o m 101 Figure 14 21 Wiring Diagram...

Page 104: ...14 Drawings P a r r I n s t r u m e n t C o m p a n y 102 Figure 14 22 Fuse Diagram...

Page 105: ...w w w p a r r i n s t c o m 103 Notes 6400 14...

Page 106: ...nseTank Empty ON RinseTank Capacity 150 Rinses Left 150 Reset RinseTank Counter RinseTime 25 Rinse FlushTime 20 ClearTime 100 of Rinse Cycles 3 Program Information and Controls Date XX XX XXXX Time XX...

Page 107: ...ls Hydrogen Entry Mode Touch Screen Oxygen Entry Mode Touch Screen Nitrogen Entry Mode Touch Screen Moisture Data Entry Controls MAD Entry Mode Touch Screen MAR Entry Mode Touch Screen Auto Sample ID...

Page 108: ...Line Setting Value Thermochemical Corrections Acid Correction STD Entered HNO3 13 Fixed Sulfur STD Off 7 Acid Correction DET Entered HNO3 13 Fixed Sulfur DET Off 7 Calculations Factors Acid Multiplie...

Page 109: ......

Page 110: ...587M R03 02 11 14...

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