Parr Instrument 6400 User Manual

Operating Instruction Manual	534M

6400

Calorimeter

6400 Calorimeter Instruction Manual
TABLE OF CONTENTS
TABLE OF CONTENTS ................................................................................................	1-1
PREFACE......................................................................................................................	1-1
Scope .........................................................................................................................	1-1
Purpose......................................................................................................................	1-2
Explanation of Symbols..............................................................................................	1-2
Safety Information ......................................................................................................	1-3
INSTALLATION.............................................................................................................	2-1
Consumables, Utilities and Power Requirements ......................................................	2-2
Electrical Connection .................................................................................................	2-2
Water Connection ......................................................................................................	2-3
Gas Connection .........................................................................................................	2-4
Bomb Exhaust Connections.......................................................................................	2-5
Communication Connections .....................................................................................	2-5
Printer Connections....................................................................................................	2-7
Balance Connections .................................................................................................	2-7
Mettler 011/012 Interface .....................................................................................	2-8
Sartorious Interface .............................................................................................	2-8
Generic Interface..................................................................................................	2-8
Bar Code Port ............................................................................................................	2-8
Computer Connections ..............................................................................................	2-9
QUICK START...............................................................................................................	3-1
OPERATION..................................................................................................................	4-1
Menu System .............................................................................................................	4-1
Menu Keys .................................................................................................................	4-1
Control Keys...............................................................................................................	4-2
Programming..............................................................................................................	4-2
Default Settings..........................................................................................................	4-2
Sample Preparation ...................................................................................................	4-3
Sample Size ...........................................................................................................	4-3
Particle Size and Moisture Content........................................................................	4-3
Sample Types ........................................................................................................	4-4
Combustion Aids ....................................................................................................	4-6
Combustion Capsules ............................................................................................	4-6
Test Process ..............................................................................................................	4-7
Loading the sample................................................................................................	4-7
Closing the bomb ...................................................................................................	4-7
Fill Cycle.................................................................................................................	4-8
Pre-Period ..............................................................................................................	4-9
Bomb Firing..........................................................................................................	4-10
Post-Period ..........................................................................................................	4-10
Cool / Rinse..........................................................................................................	4-11
Drain.....................................................................................................................	4-12
MENU DESCRIPTIONS.................................................................................................	5-1
Main Menu .................................................................................................................	5-1
Calorimeter Operation Menu......................................................................................	5-1
Temperature vs. Time Plot.........................................................................................	5-2
Temperature Plot Setup Menu ...................................................................................	5-2

	6400 Calorimeter Instruction Manual
Operating Controls Menu ...........................................................................................	5-3
Program Information and Control Menu.....................................................................	5-6
Calibration Data and Controls Menu ..........................................................................	5-8
Thermochemical Corrections Menu .........................................................................	5-11
Standardization Corrections .............................................................................	5-11
Determination Corrections................................................................................	5-11
Calculation Factors Menu ........................................................................................	5-12
Dry Calculation Menu...............................................................................................	5-13
Data Entry Controls Menu........................................................................................	5-14
Reporting Controls Menu .........................................................................................	5-16
Communication Controls Menu................................................................................	5-16
File Management Menu ...........................................................................................	5-19
Run Data File Manager ............................................................................................	5-19
Diagnostics Menu.....................................................................................................	5-20
CALCULATIONS...........................................................................................................	6-1
Corrections.................................................................................................................	6-1
Manual vs. Fixed Corrections.....................................................................................	6-2
Definitions ..................................................................................................................	6-3
ASTM, ISO and Other Methods .................................................................................	6-6
Conversion to Other Moisture Bases .........................................................................	6-7
Conversion to Net Heat of Combustion......................................................................	6-7
REPORTS......................................................................................................................	7-1
MEMORY MANAGEMENT............................................................................................	8-1
MAINTENANCE.............................................................................................................	9-1
Inspection of Critical Sealing Surfaces.......................................................................	9-1
Bomb Removal...........................................................................................................	9-2
Fuses .........................................................................................................................	9-2
Daily Maintenance......................................................................................................	9-2
Quarterly Maintenance...............................................................................................	9-2
50 to 100 Test Maintenance.......................................................................................	9-3
500 Test Maintenance................................................................................................	9-3
5000 Test Maintenance..............................................................................................	9-4
TROUBLESHOOTING.................................................................................................	10-1
Bomb Exhaust Troubleshooting ...............................................................................	10-1
Jacket Temperature Troubleshooting ......................................................................	10-3
Error List...................................................................................................................	10-3
TECHNICAL SERVICE................................................................................................	11-1
Contact Us ...............................................................................................................	11-1
Return for Repair......................................................................................................	11-1
PARTS LIST ................................................................................................................	12-1
DRAWINGS .................................................................................................................	13-1
1138 Parts Diagram Key ..........................................................................................	13-2
TABLES.......................................................................................................................	14-1

6400 Calorimeter Instruction Manual

PREFACE

Scope

This manual contains instructions for installing and operating the Parr 6400 Calorimeter. For ease of use, the manual is divided into 13 chapters.

Installation

Quick Start

Operation

Menu Descriptions

Calculations

Reports

Memory Management

Maintenance

Troubleshooting

Technical Service

Parts Lists

Drawings

Tables

Subsections of these chapters are identified in the Table of Contents.

To assure successful installation and operation, the user must study all instructions carefully before starting to use the calorimeter to obtain an understanding of the capabilities of the equipment and the safety precautions to be observed in the operation.

Additional instructions concerning the installation and operation of various component parts and peripheral items used with the 6400 calorimeter should be made a part of these instructions. Additional instructions for the optional printer are found in the respective printer package and should be made a part of this 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 unit of heat used in this manual is the International Table (IT) calorie, which is equal to 4.1868 absolute joules.

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6400 Calorimeter Instruction Manual

Purpose

Heats of combustion, as determined in an oxygen bomb calorimeter such as the 6400 Isoperibol Calorimeter, are measured by a substitution procedure in which the heat obtained from the sample is compared with the heat obtained from a standardizing material. In this test, a representative sample is burned in a high-pressure oxygen atmosphere within a metal pressure vessel or “bomb”. The energy released by the combustion is absorbed within the calorimeter and the resulting temperature change is recorded.

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. Provided
	for connection of the protective earth
	(green or green/yellow) supply system
	conductor.
	Chassis Ground. Identifies a connection
	to the chassis or frame of the equipment
	shall be bonded to Protective Earth at the
	source of supply in accordance with
	national and local electrical code
	requirements.
	Earth Ground. Functional earth
	connection. NOTE: This connection shall
	be bonded to Protective earth at the
	source of supply in accordance with
	national and local electrical code
	requirements.

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Safety Information

To avoid electrical shock, always:

1.Use a properly grounded electrical outlet of correct voltage and current handling capability.

2.Ensure that the equipment is connected to electrical service according to local national electrical codes. Failure to properly connect may create a fire or shock hazard.

3.For continued protection against possible hazard, replace fuses with same type and rating of fuse.

4.Disconnect from the power supply before maintenance or servicing.

To avoid personal injury:

1.Do not use in the presence of flammable or combustible materials; fire or explosion may result. This device contains components which may ignite such material.

2.Refer servicing to qualified personnel.

Intended Usage

If the instrument is used in a manner not specified by Parr Instrument Company, the protection provided by the equipment may be impaired.

General Specifications

Electrical ratings

115VAC, 5.0 Amps. 50/60 Hz 230VAC, 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.

Frequency: Calorimeters can be operated from either a 50 or 60 Hertz power supply without affecting their operation or calibration.

Current: The total current drawn should not exceed the rating shown on the data plate on the calorimeter by more than 10 percent.

Environmental Conditions

Operating:	15ºC to 30ºC; maximum relative humidity of 80% non-condensing.
	Installation Category II (overvoltage) in accordance with IEC 664.
	Pollution degree 2 in accordance with IEC 664.
	Altitude Limit: 2,000 meters.
Storage:	-25ºC and 65ºC; 10% to 85% relative humidity.

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6400 Calorimeter Instruction Manual

INSTALLATION

Note:

Some of the following manual sections contain information in the form of warnings, cautions and notes that require special attention. Read and follow these instructions carefully to avoid personal injury and damage to the instrument. Only personnel qualified to do so, should conduct the installation tasks described in this portion of the manual.

Each Parr 6400 Calorimeter was completely assembled and thoroughly tested prior to shipment. Unpack the calorimeter and carefully check the individual parts against the packing list. If shipping damage is discovered, save the packing cartons and report it immediately to the delivering carrier.

This apparatus is to be used indoors. It requires at least 4 square feet of workspace on a sturdy bench or table in a well-ventilated area with convenient access to an electric outlet, running water and a drain. The supply voltage must be within ± 10% of marked nominal voltage on the apparatus. The supply voltage receptacle must have an earth ground connection.

When Swagelok Tube Fittings are used, the instructions for installation are:

1.Simply insert the tubing into the Swagelok Tube 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 back-up 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.

Swagelok tubing connections can be disconnected and retightened many times. The same reliable leak-proof seal can be obtained every time the connection is remade using the simple two-step procedure.

1.Insert the tubing with pre-swaged ferrules into the fitting body until the front ferrule seats.

2.Tighten the nut by hand. Rotate the nut to the original position with a wrench. An increase in resistance will be encountered at the original position. Then

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tighten slightly with a wrench. Smaller tube sizes (up to 3/16” or 4mm) take less tightening to reach the original position than larger tube sizes.

The type of tubing and the wall thickness also has an effect on the amount of tightening required. Plastic tubing requires a minimal amount of additional tightening while heavy wall metal tubing may require somewhat more tightening. 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 causes distortion (flaring) of the lip of the tube fitting where the ferrule seats. This in turn causes the threaded portion of the body to deform. It becomes difficult to tighten the nut by hand during a subsequent re-tightening when the fitting body becomes distorted in this manner.

Consumables, Utilities and Power Requirements

The 6400 Calorimeter requires availability of oxygen, 99.5% purity, with CGA 540 connection, 2500 psig, maximum.

The 6400 Calorimeter requires availability of nitrogen or air, oil and water free, with CGA 580 connection, 2500 psig, maximum.

Approximately 16L of distilled water are required to fill the external pressurized rinse tank.

Approximately 2L of tap water, with a total hardness of 85 ppm or less, are required for filling the internal cooling reservoir.

The power requirements for the sub-assemblies of the 6400 Calorimeter are:

Calorimeter

5A @ 120 VAC

3A @ 230 VAC

Printer

(100 to 240 VAC, 50/60 Hz) 0.35 A

Electrical Connection

Plug the power line into any grounded outlet providing proper voltage that matches the specification on the nameplate of the calorimeter. Grounding is very important not only as a safety measure, but also to ensure satisfactory controller performance. If there is any question about the reliability of the ground connection through the power cord, run a separate earth ground wire to the controller chassis.

Turn the power switch to the ON position. After a short time, the Parr logo will appear on the LCD display followed by a running description of the instrument boot sequence. When the boot sequence is complete, the Main Menu is displayed.

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6400 Calorimeter Instruction Manual

Figure 1 - 6400 Calorimeter Back Panel - Label

Water Connection

Remove the cap plug on the water filling elbow and fill the internal reservoir tank with water having a total hardness of 85 ppm or less, until the water level is at the bottom of the filling elbow. The calorimeter water tank will initially accept about 2 liters.

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Fill the external rinse tank with about 16 liters of distilled water through the large opening at the top of the tank. The cover for this opening is removed by lifting up on the handle, pushing down on the lid, tilting and removing. Replace and close the cover after filling.

The two connections between the calorimeter and the 1576 Rinse Tank should be made with two pieces of 1/8” nylon pressure hose (HX0012TB024).

Figure 2 - 6400 External Plumbing

Gas Connection

Make the connections to the oxygen supply at this time. Refer to Figure 2. 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. The delivery pressure for oxygen should be set to 450 psig. To install the regulator, unscrew the protecting cap from the tank and inspect the threads on the tank outlet to be sure they are clean and in good condition. Place the ball end of the regulator in the tank outlet and draw up the union nut tightly, keeping the gages tilted slightly back from an upright position. Open the tank valve and check for leaks. The bomb must never be filled to more than 600 psig (40 atm).

Make the connections to the nitrogen supply at this time. Refer to Figure 2. 1/4” O.D. nylon pressure hose (HJ0025TB035) is used to connect the nitrogen supply. When making the nitrogen connection, a back-up wrench should be placed on the restrictor to insure a secure connection and to prevent over tightening the flow restrictor. The delivery pressure for nitrogen should be set at 80 psig. To install the regulator, unscrew the protecting cap from the tank and inspect the threads on the tank outlet to be sure they are clean and in good condition. Place the ball end of the regulator in the tank outlet and draw up the union nut tightly, keeping the gages tilted slightly back from an upright position. Open the tank valve and check for leaks.

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6400 Calorimeter Instruction Manual

Note:

A hissing sound will occur while the rinse tank is being pressurized. This is normal. Adjust the pneumatic supply regulator to 80 psig as needed.

During extended periods of inactivity, close the tank valve to prevent depleting the tank in the event of a leak. Close the tank valve prior to removing the regulator when changing tanks. Do not use oil or combustible lubricants in connection with any part of the oxygen filling system. Keep all threads, fittings and gaskets clean and in good condition.

Bomb Exhaust Connections

The exhaust and vent connections at the rear of the calorimeter, are made with the dual tube A1006DD assembly. The end of the assembly with the bomb exhaust diffuser should be placed into the 10 liter carboy (231C2). The carboy should be placed at or below the level of the calorimeter to facilitate complete draining of these lines.

Alternatively:

The A1050DD Bomb Rinse Container Assembly is provided as an accessory to the 6400 Calorimeter. See Figure 28. This device allows for complete and systematic recovery of the bomb combustion products. These combustion products include the initial line exhaust after the fill cycle and the portion expelled during the bomb rinse cycle. The Bomb Rinse Container Assembly is connected to the rear of the calorimeter, in place of the portion of the waste tube assembly that is connected to the bomb exhaust fitting. Combustion products are discharged from the bomb in two steps. The first step occurs during the initial rapid release of the residual bomb gases. The 1053DD bottle has sufficient strength and volume to deal effectively with this sudden pressure release. Gas is expelled from the four holes on the perimeter of the 1052DD bottle cap, leaving any discharged liquid in the bottle. As an additional safety measure, the bottle is supported in a 1054DD acrylic cylinder which serves to keep the bottle upright and contained in the unlikely event the bottle ruptures. At the end of the bomb exhaust step the aqueous combustion products reside in the bomb, associated tubing as well as the 1053DD bottle. The bomb rinse step flushes these combustion products from the bomb and the tubing into the 1053DD bottle. The bottle can then be unscrewed from the assembly and capped, until the sample is to be analyzed. Some users find it useful to add the contents of the rinsed combustion capsule to the washings collected in the bottle. Three 1053DD bottles are provided with the assembly. Additional bottles may be ordered separately from Parr.

Communication Connections

There are three RS-232 serial ports at the rear of the calorimeter. These ports are designated Terminal, Printer and Balance. The pin-out of these three ports are identical and can be found in Table 1.

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6400 Calorimeter Instruction Manual

Table 1 - 6400 Calorimeter Serial Ports Pin-Out

9 pin D Connector Pin #	Description	Direction
		(6400 – External Device)
2	Received Data	Í
3	Transmitted Data	Î
4
5	Signal Ground	Í Î
6
7	Ready to Send (RTS)	Î
8	Clear to Send (CTS)	Í

The RS232 balance port is a female port whereas the RS232 printer port is a male port. The 6400 Calorimeter is also equipped with an RJ45 Ethernet port for connection to a computer. Before making any of these connections, the data transmission rate of the Calorimeter and the printer, balance or computer must be matched. Generally the baud rates on either device can be changed to achieve this match.

The 6400 will also allow the user to specify the IP addresses of one or more Balance Interface devices on the network by selecting the Network Data Device menu in the Communications Controls menu. Balance Interface devices are polled from device 1 to 15 for sample and / or spike weights when the weight entry mode is set to Network.

Figure 3 - 6400 Calorimeter Peripherals

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6400 Calorimeter Instruction Manual

Multiple Alternate Configurations

Printer Connections

The printer port settings are on the Communication Controls Menu: Printer Port Communications Menu. The default parameters for the 6400 are set up for use with the Parr 1757 Printer. Table 1 identifies and describes the pin-out for the RS-232 port.

Balance Connections

The 6400 Calorimeter supports input from the multiple balance types. Additionally, a generic input driver is provided for communications with balances that do not conform to the eight supported protocols. A new feature supported by all balance input drivers is the ability to change the expected number of characters in the data field. The number of data characters indicated for each of the drivers, below, are default values. This feature virtually eliminates the need for balance input drivers to be re-written in the event the balance manufacturer elects to alter the output string of a balance when new models are introduced.

The format of an unknown balance can be determined by logging the balance output to the printer attached to the calorimeter. Those protocols which send a command string to the balance will do so while logging is active. In order for the logging to produce meaningful results, the cable connecting the balance to the balance input port of the calorimeter must be correctly wired or configured. In addition, the specifics of the data frame, such as the baud rate, # of data bits, parity, # of stop bits and handshaking (if used) must be the same for both the balance and the calorimeter.

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6400 Calorimeter Instruction Manual

Mettler 011/012 Interface

The ID field must contain “S_” to indicate a stable mass. The data field contains the current mass, right justified, with a decimal point. The balance should be configured to send continuously.

Sartorious Interface

The polarity field must contain either a “+” or a space. Leading zeros in the data field are blanked, except for the one to the left of the decimal point. The stability field must contain “g_” for the calorimeter to accept a mass. The balance should be configured to transmit data upon receipt of the following command string:

[ESC] P [CR] [LF]

Field	Length
ID	2
space	1
data	9
space	1
g	1
CR	1
LF	1

Field	Length
polarity	1
space	1
data	8
space	1
stability	2
CR	1
LF	1

Note:

The automatic data output option should not be used.

Generic Interface	Field	Length
The data field should consist of 9	data	8
numeric characters (0 through 9, +, -	CR	1

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.

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. Select the “Program Information and Control” key from the Main Menu. Next, select “Feature Key” and enter the feature key purchased from Parr Instrument Company into the instrument by using the touchpad. Pressing the key labeled “ABC” allows the user to switch from upper case letters, to lower case letters, to numerals, and finally to symbols. A CD containing all the necessary documentation and setup information for using both the scanner and the printer is provided at the time of purchase. A PC based program used for printing bar coded labels is also provided on this CD.

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6400 Calorimeter Instruction Manual

Computer Connections

If the 6400 Calorimeter is to be connected to a computer, the Ethernet connection should be used. Test data can be transferred to an Ethernet network connected computer using the FTP File Transfer Protocol. First, you must know the IP address of the network-connected calorimeter. The network DHCP (Dynamic Host Configuration Protocol) server provides this address shortly after the calorimeter is turned on. The address can be seen on the Software & Hardware Info” screen, under Program

Info and Control Menu (see the example screenshot). Users who don’t have a network infrastructure can create a simple network by connecting a router with DHCP server capability to the calorimeter using an ordinary CAT 5 network cable. The calorimeter should be connected 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 without a WAN connection, the primary DNS address of the router (WAN setup) must be set to the IP address of the router found on the LAN setup page. Other routers behave differently in the absence of a WAN connection. Providing an active upstream connection to the WAN port of most routers generally minimizes the use of any obscure setup configurations. An FTP enabled web browser can be used to access stored test data. The URL is of the following form:

ftp://root:rootroot@192.168.0.125/../flash/data/

In this case, 192.168.0.125 is the IP address of the calorimeter.

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6400 Calorimeter Instruction Manual

The following screenshot illustrates the contents of the calorimeter data directory as presented by a web browser.

You can drag and drop or copy and paste test data files (with the csv suffix) from the web browser window to any convenient folder or directory on the PC.

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6400 Calorimeter Instruction Manual

The calorimeter offers a web server service. Test reports can be viewed with a web browser using a URL of the following form: http://192.168.0.125, where 192.168.0.125 is the IP address of the calorimeter.

Clicking on the Sample Data tab displays a list of reports currently in the instrument memory.

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Clicking on any given report will provide a display similar to the following:

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QUICK START

1.Turn on the heater and pump in the Calorimeter Operation menu. Allow at least 20 minutes for the calorimeter to warm up.

2.Initiate a pretest to run the calorimeter through the fill and cool/rinse cycles. This function is used to pre-condition the calorimeter if it has been sitting idle for an extended period of time (greater than 15 minutes).

3.Prepare and weigh the sample to 0.0001g.

4.Gently tap capsules that contain powdered samples to compact the material. (Pellets are easier to handle than loose samples and they burn slower in the bomb, thereby reducing the chances for incomplete combustion).

5.Carefully place the capsule into the capsule holder, attach 10 cm of ignition thread and install the bomb head in the calorimeter.

6.Close the calorimeter cover making sure that the latch is engaged.

7.Select determination or standardization as appropriate on the Calorimeter Operation page, by toggling the operating mode key. Press the Start Key. The calorimeter will now prompt the operator for Bomb ID number, sample ID number, sample weight and spike weight in accordance with the instructions set into the operating controls page.

8.The calorimeter will now take over and conduct the test. During the time it is establishing the initial equilibrium, it will display PREPERIOD on the status bar. Just before it fires the bomb, it will sound a series of short beeps to warn the user to move away from the calorimeter. Once the bomb has been fired, the status bar will display POSTPERIOD. The calorimeter will check to make certain that a temperature rise occurs and will then look for the final equilibrium conditions to be met. If it fails to meet either the initial or final equilibrium conditions, or if it fails to detect a temperature rise within the allotted time, the test will terminate and advise the user of the error.

9.At the conclusion of the test, the calorimeter will signal the user.

10.Open the cover and remove the head. Examine the interior of the bomb for soot or other evidence of incomplete combustion. If such evidence is found, the test will have to be discarded.

11.Titrate the bomb washings with a standard sodium carbonate solution using methyl orange, red or purple indicator. A 0.0709N sodium carbonate solution is recommended for this titration to simplify the calculation. This is prepared by dissolving 3.76 grams of

Na2CO3 in the water and diluting to one liter. NaOH or KOH solutions of the same normality may be used.

12.Analyze the bomb washings to determine the sulfur content of the sample if it exceeds 0.1%. Methods for determining sulfur are discussed in Analytical Methods for Oxygen Bombs, No. 207M.

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OPERATION

Menu System

All configurations and operations are handled by a menu-driven system operated from the bright touch screen display. The settings and controls are organized into ten main sections as displayed on the MAIN MENU.

Note:

Keys with a “double box” in the upper left hand corner lead to sub-menus.

Menu Keys

The controls that change the data field information in the menus will be one of the following:

1.Toggles. These data fields contain ON/OFF or YES/NO choices. Simply touching the key on the screen toggles the choice to the other option. The current setting is displayed in the lower right corner of the key.

2.Option Selection. These data fields contain a list of options. Touching the key on the screen steps the user through the available choices. The current setting is displayed in the lower right corner of the key.

3.Value Entry Fields. These data fields are used to enter data into the Calorimeter. Touching the key on the screen brings up a sub-menu with a key pad or similar screen for entering the required 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.

4.Data Displays. Most of these keys display values that have been calculated by the calorimeter and are informational only. Certain ones can be overridden by the user entering a desired value through a sub-menu. The value is displayed in the lower right corner of the key.

Note:

Some keys will respond with an opportunity for the user to confirm the specified action to minimize accidental disruptions to the program and/or stored data.

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Control Keys

There are five control keys which always appear in the right column of the primary displays. These keys are unavailable when they are gray instead of white.

1.Escape. This key is used to go up one level in the menu structure.

2.Main Menu. This key is used to return to the main menu touch screen from anywhere in the menu structure.

3.Start. This key is used to start a test.

4.Report. This key is used to access the test results stored in the calorimeter, to enter thermochemical corrections, and to initiate a report on the display, printer or attached computer.

5.Help. This key is used to access help screens related to the menu currently displayed on the touch screen.

Programming

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. Numerous provisions are included to permit the use of other reagent concentrations, techniques, combustion aids and short cuts appropriate for the user’s work.

Note:

Changes to the program are made by use of the menu structure. Any of these items can be individually entered at any time to revise the operating program.

Default Settings

Units are preprogrammed with default settings. See Table 2 for a listing of the factory default settings. A more in-depth explanation of these parameters is found on the corresponding parameter group help pages. These default settings remain in effect until changed by the user. Should the user ever wish to return to the factory default settings, go to the Program Info and Control Menu, User/Factory Settings, touch Reload Factory Default Settings and YES. Non-volatile memory is provided to retain any and all operator initiated program changes; even if power is interrupted or the unit is turned off. If the unit experiences an intentional or unintentional “Cold Restart”, the controller will return to the last known settings.

The default parameters of the 6400 calorimeter can be changed to guarantee that the calorimeter, when cold restarted, will always be in the desired configuration before beginning a series of tests. Users who wish to permanently revise their default settings may do so using the following procedure:

•Establish the operating parameters to be stored as the user default settings.

•Go to the Program Info and Control Menu, User/ Factory Settings, User Setup ID, and enter the desired User Setup ID.

•Select Save User Default Settings

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To re-load the user default setting, go to the Program Info and Control Page, User/Factory Settings, Re-load User Default Settings, and YES.

Sample Preparation

Sample Size

To stay within safe limits, the bomb should never be charged with a sample which will release more than 8000 calories when burned in oxygen. The initial oxygen pressure is set at 30 atmospheres (450 psig). 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. To avoid damage to the bomb and calorimeter, and possible injury to the operator, it should be a standing rule in each laboratory that the bomb must never be charged with more than 1.5 grams of combustible material.

When starting tests with new or unfamiliar materials, it is always best to use samples of less than 0.7 grams with the possibility of increasing the amount if preliminary tests indicate no abnormal behavior and sample will not exceed the 8000 calorie limit.

Samples containing sulfur should contain no more than 50 mg of sulfur and have a calorific value of at least 9000 BTU/lb.

Samples containing chlorine should be spiked to insure that sample contains no more than 100 mg of chlorine and liberates at least 5000 calories

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. Compression into a pellet is recommended because the pressure developed during combustion can be reduced as much as 40% when compared to the combustion of the material in the powder form. In addition to giving controlled burn rates, the formation of pellets from sample material keeps the sample in the fuel capsule during combustion.

Materials, such as coal, burn well in the as-received or air-dry condition, but do not burn completely dry samples. A certain amount of moisture is desirable in order to control the burning rate. Moisture content up to 20% can be tolerated in many cases, but the optimum moisture is best determined by trial 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.

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Sample Types

Because of the difference in combustion characteristics of the many different materials which may be burned in an oxygen bomb, it is difficult to give specific directions which will assure complete combustions for all samples.

The following fundamental conditions should be considered when burning samples:

•Some part of the sample must be heated to its ignition temperature to start the combustion and, in burning, it must liberate sufficient heat to support its own combustion regardless of the chilling effect of the adjacent metal parts.

•The combustion must produce sufficient turbulence within the bomb to bring oxygen into the fuel cup for burning the last traces of the sample.

•A loose or powdery condition of the sample which will permit unburned particles to be ejected during a violent combustion.

•The use of a sample which contains coarse particles will not burn readily. Coal particles which are too large to pass a 60 mesh screen may not burn completely.

•The use of a sample pellet which has been made too hard or too soft can cause spalling and the ejection of unburned fragments.

•The bottom of the cup should always be at least one-half inch above the bottom of the bomb or above the liquid level in the bomb to prevent thermal quenching.

•If the moisture, ash and other non combustible material in the sample totals approximately 20% or more of the charge, it may be difficult to obtain complete combustion. This condition can be remedied by adding a small amount of benzoic acid or other combustion aid.

Foodstuffs and Cellulosic Materials

Fibrous 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 such as mineral oil to retard the burn rate and avoid development of high pressures. Partial drying may be necessary if the moisture content is too high to obtain ignition, but if the sample is heat sensitive and cannot be dried, a water soluble combustion aid such as ethylene glycol can be added to promote ignition. Material such as Napthalene should not be burned in loose powder form but should be formed into a pellet.

Coarse Samples

In most cases it may be necessary to burn coarse samples without size reduction since grinding or drying may introduce unwanted changes. There is no objection to this if the coarse sample will ignite and burn completely. Whole wheat grains and coarse charcoal chunks are typical of materials which will burn satisfactorily without grinding and without additives or a special procedure.

Corrosive Samples

The 1138 bomb is made from alloy 20; a special niobium stabilized stainless steel selected for its resistance to the mixed nitric and sulfuric acids produced during the combustion process. The 1138CL is made from the halogen resistant Hastelloy G30™. Hastelloy 30™ is an alloy rich in cobalt and molybdenum and is able to resist the corrosive effects of free chlorine and halogen acids produced when burning samples with significant chlorine content. While no alloy will completely resist the corrosive atmospheres produced when burning samples containing halogen compounds; users

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who intend to test these materials are urged to select the 1138CL Bomb. These bombs are 250 mL in volume and are rated to a maximum working pressure of 2000 psi. The bombs are hydrostatically tested to 3000 psi and the sample range is ~1g or 5000 – 8000 calories.

Explosives and High Energy Fuels

Materials which release large volumes of gas which detonate with explosive force or burn with unusually high energy levels, should not be tested in this calorimeter. Rather, they should be tested in a model 6100 or 6200 Calorimeter which can be equipped with an 1104 High Strength Oxygen Bomb designed specifically for these types of samples.

Volatile Sample Holders

Volatile samples are defined as one with an initial boiling point below 180ºC per ASTM D-2. 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. The seal obtained after pressing this disc firmly against the rim of the cup with a flat blade will be adequate for most volatile samples. The tape used for this purpose should be free of chlorine and as low in sulfur as possible. Borden Mystic Tape, No. M-169-C or 3M Transparent Tape, No. 610, are recommended for this purpose. The 3M Transparent Tape can be ordered through Parr, Part No. 517A.

Figure 4 - Volatile Sample Technique

The weight of the tape disc must be determined separately and a correction applied for any elements in the tape which might interfere with the determination. The approximate Heat of

Combustion of the tape is 6300 cal/g. An actual amount should be determined by running a blank test with tape alone using a sample weighing 1.0 gram. The compensation for heat of tape may be done through the spike option; see Spike Controls, Heat of Combustion of Spike.

Note:

Tape should always be stored in a sealed container to minimize changes in its moisture and solvent content.

Use the following procedure when filling and handling 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 against the metal rim. Also cut and attach a small flag to the disc (see Figure 4).

2.Puncture the tape at a point below the flag, then re-weigh the empty cup with its tape cover.

3.Add the sample with a hypodermic syringe; close the opening with the flag and re-weigh the filled cup.

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4.Set the cup in the capsule holder and arrange the auxiliary fuse so that it touches the center of the tape disc.

5.Just before starting the test, prick the disc with a sharp needle to make a small opening which is needed to prevent collapse of the disc when pressure is applied.

6.Fill the bomb with the usual oxygen charging pressure.

7.The calorimeter will fire the bomb and complete the test in the usual manner.

Combustion Aids

Some samples may be difficult to ignite or they may burn so slowly that the particles become chilled below the ignition point before complete combustion is obtained. In such cases white oil or other suitable material of known purity can be mixed with the sample. Ethylene glycol, butyl alcohol or decalin may be used for this purpose.

Note:

It must be remembered, that a combustion aid adds to the total energy released in the bomb and the amount of sample may have to be reduced to compensate for the added charge.

When benzoic acid is combusted for standardization runs, it should be in the form of a pellet to avoid possible damage to the bomb which might result from rapid combustion of the loose powder.

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 and platinum alloyed with 3-1/2% rhodium.

Stainless steel capsules (43AS) are furnished with each calorimeter. The stainless steel capsules will acquire a dull gray finish after repeated use in an oxygen bomb due to the formation of a hard, protective oxide film. This dull finish not only protects the capsule, but it also promotes combustion and makes it easier to burn the last traces of the sample. New capsules are heated in a muffle furnace at 500ºC for 24 hours to develop this protective coating uniformly on all surfaces. This treatment should be repeated after a capsule has been polished with an abrasive to remove any ash or other surface deposits. Heating in a muffle is also a good way to destroy any traces of carbon or combustible matter which might remain in the capsule from a previous test. Capsules should be monitored for wear. Do not use the capsule if the wall or base thickness is less than 0.025”.

Note:

After heating, place the capsules in a clean container and handle them only with forceps when they are removed to be weighed on an analytical balance.

When combusting samples that contain metal particles such as aluminum or magnesium, the non-metallic (fused silica) 43A3 Capsule is required.

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When superior corrosion resistance is needed, the Platinum Rhodium 43A5 Capsule is required.

Test Process

Loading the sample

Prepare and weigh the sample to 0.0001g. Gently tap capsules that contain powdered samples to compact the material. (Pellets are easier to handle than loose samples and they burn slower in the bomb, thereby reducing the chances for incomplete combustion).

Carefully place the capsule into the capsule holder. A cotton thread (845DD2) is used as an auxiliary fuse to ignite the sample. Remove any moisture from the heating wire prior to attaching the cotton thread.

Figure 5 - Cotton Thread Assembly

Four inches of thread is recommended for this auxiliary thread which is looped over the heating wire, doubled on itself, twisted to form a single strand and fed into the sample cup to lay on the sample. When contact is made through the heating wire, the thread will ignite, drop into the sample cup and ignite the sample. One spool of thread, part number 845DD, is 563 yards. Part number 845DD2 contains approximately 1000 pieces of thread pre-cut to 4 inches.

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.

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Notice that the bomb head grounding lug extends beyond the outside diameter of the bomb head. A slot for this lug is cut into the top of the calorimeter bucket which holds the bomb cylinder. Position this lug approximately 20 degrees to the operators right and slide the head into the cylinder and push it down as far as it will go. Now rotate the bomb head 20 degrees to the left until the lug contacts the left edge of the cut out and is pointed to the front of the calorimeter.

Fill Cycle

Once the calorimeter is started and the cover is closed, the fill sequence begins.

Figure 6 - Bucket Fill Flow Diagram

1. The calorimeter checks the bomb ignition circuitry for continuity.

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2.The water fill solenoid opens and water is pumped from the internal tank into and through the bucket that surrounds the bomb. Overflow from the bucket is returned to the closed water tank. Because the jacket and bucket are both filled with water from the closed water tank, initial equilibrium will be reached quickly.

3.The oxygen fill solenoid is opened and oxygen is added slowly to the bomb to bring its pressure to approximately 30 atm.

Pre-Period

At the completion of the fill sequence, the pre-period begins.

Figure 7 - 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

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continues to circulate from the closed water system through the jacket surrounding the bucket.

2.The oxygen filling valve closes and the pressure in the filling line is vented. The automatic check valve at the top of the bomb closes and isolates the bomb from the oxygen filling line.

3.The controller monitors the operating temperature until it confirms that the initial equilibrium has been established.

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 7, from the preperiod through the bomb firing and post-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-period begins. See Figure 7.

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.

2.Once the final temperature rise is determined, it is recorded with the test results.

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Cool / Rinse

At the completion of the post-period, the rinse and cool sequence begins.

Figure 8 - Rinse & Cool Flow Diagram

1.Chilled water is circulated through the bucket to cool the bomb to the starting temperature.

2.The release valve in the bottom of the bomb is opened and the residual pressure is released through the bomb exhaust line.

3.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. The bomb rinse water is released to the wash bottle.

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