Sample_587M_Parr_6400-Calorimeter-After-10-2010-Inst.pdf

587M

Automatic Isoperibol Calorimeter

Operating Instruction Manual For models produced after October 2010

SAMPLE

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Table of Contents6400

Preface 4

Scope 4 Related Instructions 4 Purpose 4 Explanation of Symbols 5 Safety Information 5 Intended Usage 5 General Specifications 6 Environmental Conditions 6 Provisions for Lifting and Carrying 6 Cleaning & Maintenance 6

Chapter 1 8

Installation 8

Environmental Conditions 8 Swagelok Tube Fittings 8 Required Consumables, Utilities and Power Requirements 9 Electrical Connection 9 Front Panel Meter 9 Water Connection 11 Gas Connection 12 Bomb Exhaust Connections 12 Communication Connections 13 Printer Connections 13 Balance Connections 13

Chapter 2 16

Quick Start 16

Initial Fill 16 Quick Start 16

Chapter 3 18

Operation 18

Menu System 18 Menu Keys 18 Control Keys 18 Programming 18 Default Settings 19 Sample Preparation 19 Test Process 22

Closing the bomb 22 Fill Cycle 23 Pre-Period 24 Bomb Firing 25 Post-Period 25 Cool/Rinse 26 Drain 27

Chapter 4 28

Menu Descriptions 28

Main Menu 28 Calorimeter Operation Menu 28

Temperature vs. Time Plot 29 Temperature Plot Setup Menu 29

Operating Controls Menu 30 Spiking Controls 30 Bomb Rinse Tank Controls 31

Program Information and Control Menu 32 Software & Hardware Info 32 User/Factory Settings 33

Calibration Data and Controls Menu 34 Bomb 1 35 Control Plot Chart Plot 35

Thermochemical Corrections Menu 36 Calculation Factors Menu 37 Net Heat/Dry Heat Factors 38

Data Entry Controls Menu 38 Net Heat Data Entry Controls 38 Auto Sample ID Controls 39 Moisture Data Entry Controls 39 Preweigh Sample ID Controls 40

Reporting Controls Menu 40 Communication Controls Menu 41

Balance Port Communications 41 Balance Port Settings 41

File Management Menu 42 Run Data File Manager 43

Diagnostics Menu 43 Data Logger Controls 44 Data Log Items 44 User Defined Buttons 45 I/O Diagnostics: 45

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

Table of Contents

Chapter 5 46

Reports 46

Chapter 6 48

Standardizations 48

Standardizing the Calorimeter 48 Standard Materials 48 Automatic Statistical Calculations 48

Chapter 7 52

Calculations 52

Calculating the Heat of Combustion 52 General Calculations 52 Thermochemical Corrections 52 ASTM and ISO Methods Differ 53 Thermochemical Calculation Details 54 Acid and Sulfur Corrections 54 ASTM Treatment for Acid and Sulfur 56 ISO Calculations 56 Spiking Samples 57 Conversion to Other Moisture Bases 57 Conversion to Net Heat of Combustion 57

Chapter 8 58

Computer Communications 58

Computer Connections 58 Advanced Network Options 59 Samba Server Feature (Optional) 59 Bar Code Port 66

Chapter 9 68

Memory Management 68

Clearing Memory 68 Removable SD Memory 68 USB Flash Drive 68

Chapter 10 70

Maintenance 70

Inspection of Critical Sealing Surfaces 70 Bomb Removal 70 Fuses 71 Daily Maintenance 71 Quarterly Maintenance 71 50 to 100 Test Maintenance 71 500 Test Maintenance 71 5000 Test Maintenance 72 6400 Maintenance Checklist 73

Chapter 11 74

Troubleshooting 74

Bomb Exhaust Troubleshooting 74 Jacket Temperature Troubleshooting 75 Error List 76

Chapter 12 78

Technical Service 78

Return for Repair 78

Chapter 13 80

Parts Lists 80

Principal Assemblies in Calorimeter 80 A1250DD2 Controller Assembly 80 A1265DD Bucket and Stirrer Tube Assembly 80 A1255DD Bucket Stirrer Assembly 81 A1266DD Cover Assembly 81 A1457DD Accessory/Installation Kit 81

Chapter 14 82

Drawings 82

Chapter 15 104

Tables 104 w w w . p a r r i n s t . c o m

Table of Contents6400

Figures

Figure 1-1 Swagelok Tube Fittings 8 Figure 1-2 6400 Calorimeter Back Panel 10 Figure 1-3 6400 External Plumbing 11 Figure 1-4 6400 Calorimeter Peripherals 14 Figure 1-5 Multiple Alternate Configurations 14 Figure 3-1 Volatile Sample Technique 21 Figure 3-2 Cotton Thread Assembly 22 Figure 3-3 Bucket Fill Flow Diagram 23 Figure 3-4 Pre-Period/Post-Period Flow Diagram 24 Figure 3-5 Rinse & Cool Flow Diagram 26 Figure 3-6 Drain Flow Diagram 27 Figure 14-1a 1138 Parts Diagram 82 Figure 14-1b 1138 Parts Diagram Key 83 Figure 14-2 A1450DD Bomb Head Assembly, View 1 84 Figure 14-3 A1450DD Bomb Head Assembly, View 2 85 Figure 14-4 6400 Bucket Assembly 86 Figure 14-5 6400 Air Can Assembly, Cutaway Left 87 Figure 14-6 6400 Air Can Assembly, Cutaway Front 88 Figure 14-7 6400 Cutaway Right 89 Figure 14-8 6400 Cutaway Left 90 Figure 14-9 6400 Cover Open, View 1 91 Figure 14-10 6400 Cover Open, View 2 92 Figure 14-11 6400 Internal Plumbing Diagram 93

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 Values in cal/g When Benzoic Acid is Used as a Test Sample 50 Table 6-3 Calorimeter Control Limit Values in BTU/lb When Benzoic Acid is Used as a Test Sample 51 Table 8-1 6400 Data File Naming Convention 66 Table 8-2 6400 Calorimeter Run Data Template 67 Table 15-1 Factory Default Settings 104 Table 15-2 Settings for ISO & BSI Methods 106

Figure 14-12 A1251DD Oxygen Solenoid Assembly 94 Figure 14-13 A1447DD Water Solenoid Assembly 95 Figure 14-14 A1456DD Rinse Valve Assembly 96 Figure 14-15 6400 Water Tank and Jacket Cooling Solenoid 96 Figure 14-16 A1448DD Temperature Control Assembly 97 Figure 14-17 A1050DD Rinse Collection Assembly 97 Figure 14-18 A1455DD Propeller Assembly 98 Figure 14-19 A1268DD Stirrer Motor and Mount 98 Figure 14-20 Fuse Diagram 99 Figure 14-21 A1250DD2 Control Schematic 100 Figure 14-22 Power Input and Cooling Wiring 101 Figure 14-23 Ignition Wiring Diagram 102 Figure 14-24 Heater/Pump Power Wiring Diagram 102 Figure 14-25 Solenoid Harness Wiring Diagram 103

Preface

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PREFACE

Scope

This manual contains instructions for installing and operating the Parr 6400 Calorimeter. For ease of use, the manual is divided into 15 chapters.

1. Installation

2. Quick Start

3. Operation

4. Menu Descriptions

5. Reports

6. Standardizations

7. Calculations

8. Computer Communications

9. Memory Management

10. Maintenance

11. Troubleshooting

12. Technical Service

13. Parts Lists

14. Drawings

15. 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 under-standing of the capabilities of the equipment and the safety precautions to be observed in the operation.

Related Instructions

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. Addi-tional 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 calorie, which is equal to 4.1868 absolute joules.

Purpose

Heats of combustion, as determined in an oxygen bomb calorimeter such as the 6400 Automatic Isoperibol Calorimeter, are measured by a substitu-tion 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 atmo-sphere 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.

Note About Nomenclature: Historically, burning a sample enclosed in a high pressure oxygen environment is known as Oxygen Bomb Calorimetry and the vessel containing the sample is known as an Oxygen Bomb. The terms bomb and vessel are used interchangeably.

Product Registration & Customer Satisfaction Parr’s Product Registration and Customer Satisfaction Survey can be found by visiting our website at: www.parrinst.com/support/product-registration Register your equipment with us so you can receive:

Notification of Product Updates Free Software Upgrades New Product Information

Please complete our Customer Satisfaction Survey so that we may better serve you. Your feedback helps us improve our products and customer service.

Preface6400 w w w . p a r r i n s t . c o m 5

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 pro-vided by the equipment may be impaired.

Explanation of Symbols

I On Position

O Off Position

~ Alternating Current

This CAUTION symbol may be present on the Product Instrumenta-tion 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 precau-tions for handling electrostatic sensitive devices.

Protective Earth (PE) terminal. Provided for connection of the protec-tive 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. This connection shall be bonded to Protective earth at the source of supply in accordance with national and local electrical code requirements.

Preface

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General Specifications

Electrical Ratings 120VAC, 5.0 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.

Frequency: Calorimeters can be operated from either a 50 or 60 Hertz power supply without affect-ing the operation or calibration.

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

Environmental Conditions

Operating: 15 ºC to 30 ºC; 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 Limit: 2,000 meters.

Storage: -25 ºC to 65 ºC; 10% to 85% relative humidity.

Provisions for Lifting and Carrying

Before moving the instrument, disconnect all con-nections from the rear of the apparatus. Lift the instrument by grabbing underneath each corner.

Cleaning & Maintenance

Periodic cleaning may be performed on the exterior surfaces of the instrument with a lightly dampened cloth containing mild soap solution. All power should be disconnected when cleaning the instru-ment. There are no user serviceable parts inside the product other than what is specifically called out and discussed in this manual. Advanced trouble-shooting instructions beyond the scope of this manual can be obtained by calling Parr Instrument Company in order to determine which part(s) may be replaced or serviced.

Customer Service

Questions concerning the installation or operation of this instrument can be answered by the Parr Customer Service Department:

Fax: 1-309-762-9453 E-mail: parr@parrinst.com www.parrinst.com w w w . p a r r i n s t . c o m 7

Notes 6400

1 Installation

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CHAPTER 1

Installation

Note: Some of the following manual sections contain information in the form of warnings, cautions and notes that require special at-tention. Read and follow these instructions carefully to avoid personal injury and dam-age to the instrument. Only personnel quali-fied to do so, should conduct the installation tasks described in this portion of the manual.

Environmental Conditions

The 6400 Calorimeter is completely assembled and given a thorough test before it is shipped from the factory. If the user follows these instructions, instal-lation of the calorimeter should be completed with little or no difficulty. If the factory settings are not disturbed, only minor adjustments will be needed to adapt the calorimeter to operating conditions in the user’s laboratory.

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.

Swagelok Tube Fittings

When Swagelok Tube Fittings are used, the instruc-tions 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 finger-tight.

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 revo-lution and continue to the 9 o’clock position.

4. For 3/16” and 4mm or smaller tube fittings, tight-en the Swagelok nut 3/4 turns from finger-tight.

Figure 1-1 Swagelok Tube Fittings

Swagelok tubing connections can be disconnected and retightened many times. The same reliable leak-proof seal can be obtained every time the connec-tion 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 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.

Installation6400 1 w w w . p a r r i n s t . c o m 9

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 ad-ditional tightening while heavy wall metal tubing may require somewhat more tightening. In general, the nut only needs to be tightened about 1/8 turn beyond finger tight where the ferrule seats in order to obtain a tight seal.

Over tightening the nut should be avoided. 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.

Required Consumables, Utilities and Power Requirements

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

The 6400 Calorimeter requires availability of ni-trogen or air, oil and water free, with appropriate connection, 2500 psig, maximum.

Approximately 16L of distilled water 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 reservoir.

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

Calorimeter

5.0 Amps @ 120 VAC

3.0 Amps @ 240 VAC

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

Electrical Connection

Plug the power line into any grounded outlet provid-ing 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 in-strument boot sequence. When the boot sequence is complete, the Main Menu is displayed.

Front Panel Meter

The panel meter on the front of the calorimeter controls the temperature of the water in the internal cooling resorvoir. The setpoint is locked at 15 °C.

A red light will flash in the upper left corner of the display when the water is being cooled.

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Figure 1-2 6400 Calorimeter Back Panel

ETHERNET SD 2 SD 1

INSERT CARD FACE DOWN

A1435DD_S16 R0

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Water Connection

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

Fill the external rinse tank with about 16 liters of distilled water through the large opening at the top

Figure 1-3 6400 External Plumbing 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 connection between the calorimeter and the A1589DD Rinse Tank should be made with a piece of 1/8” nylon pressure hose (HX0012TB024). See Figure 1-3 below.

Tube No. Part No. Description Max Length 1 HX0012TB024 1/8” OD, Nylon 5 ft 2 HJ0025TB035 1/4” OD, Nylon 5 ft 3 HX0012TB024 1/8” OD, Nylon 5 ft 4 HX0012TB024 1/8” OD, Nylon 10 ft 5 HX0038TB062 3/8” OD, Bev-A-Line 10 ft

CALORIMETER

VENT 4

3EXHAUSTOR

PLASTIC CONTAINER

(231C2)

RINSE CONTAINER ASSEMBLY

(A1050DD)

BOTTLE SUPPORT

(1054DD)

OXYGEN

(359VB)

IN-LINE FILTER

OXYGEN REGULATOR

ASSEMBLY (450 PSIG)

(A570DD)

RINSE WATER RINSE

TANK

A1589DD

PNEUMATIC SUPPLY

NITROGEN REGULATOR

ASSEMBLY (80 PSIG)

(A812DD)

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Gas Connection

Make the connections to the oxygen supply at this time using the A570DD Oxygen Regulator.

Refer to Figure 1-3. 1/8” O.D. nylon pressure hose (HX0012TB024) is used to connect the oxygen supply. The inlet connection incorporates a flow restrictor just behind the inlet connection. When making the oxygen connection, a back-up wrench should be placed on the restrictor to insure a secure connection and to prevent over tightening the flow restrictor. 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. 1/4” O.D. nylon pressure hose (HJ0025TB035) is used to connect the A812DD Nitrogen Regulator to the A1589DD Rinse Tank. When making the nitro-gen connection, a back-up wrench should be placed on the fitting to insure a secure connection and to prevent over tightening the flow restrictor. The de-livery 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 condi-tion. 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.

Note: A hissing sound will occur while the rinse tank is being pressurized. This is nor-mal. 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, 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 will exhaust through the relief valve. Once the pressure has equal-ized remove the lid to refill the rinse tank.

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 com-plete draining of these lines.

Alternatively:

The A1050DD Bomb Rinse Container Assembly is available as an accessory to the 6400 Calorimeter.

See Figure 14-17. 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 dis-charged 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 sepa-rately from Parr.

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Mettler 011/012 Interface The ID field must contain “S_” to indicate a stable mass. The data field con-tains the current mass, right justified, with a decimal point. The balance should be configured to send con-tinuously.

Sartorius Interface The polarity field must con-tain 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]

Note: The automatic data output option should not be used.

Generic Interface The data field should con-sist 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 charac-ters 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.

Communication Connections

There is a Universal Serial Bus (USB) port at the rear of the calorimeter.

The USB port is used to connect to external devices such as a printer or balance. Multiple devices can be attached by installing a USB hub.

The 6400 Calorimeter is also equipped with an RJ45 Ethernet port for connection to a computer.

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.

Printer Connections

The printer settings are on the Communication Controls Menu. The default parameters for the 6400 are set up for use with the Parr 1758 Printer.

Balance Connections

The 6400 Calorimeter supports input from 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 driv-ers 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 deter-mined 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 calo-rimeter 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.

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

Field Length data 8

CR 1

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Figure 1-4 6400 Calorimeter Peripherals

Figure 1-5 Multiple Alternate Configurations

COMPUTER PRINTER

BALANCE

ROUTER, SWITCH, OR HUB

PROXIMATE

INTERFACE

PROXIMATE

INTERFACE

(Acting as ADL or TM)

PRINTER

BALANCE

USB HUBSAMPLE

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Notes 6400 1

2 Quick Start

P a r r I n s t r u m e n t C o m p a n y16

CHAPTER 2

Quick Start

Initial Fill

When you first fill the calorimeter with water the main reservoir will be filled. There is also a cooling water reservoir that is filled from the main reservoir.

Once the calorimeter has been filled with water and all external connections made:

1. Turn on the calorimeter.

2. Once at the Main Menu go to the Calorimeter Op-eration screen and turn ON the heater and pump.

Water should start to circulate in the tubing.

3. Press Escape to get back to the Main Menu. Then press Diagnostics and then I/O Diagnostics.

4. Use the side arrow keys(< >) until the description reads H2O Cool.

5. Unlock and remove the vessel head.

6. Press “1” to turn on the H2O Cool. You should hear a click and then gurgling coming from the bomb cylinder.

7. Once the gurgling stops turn off the H2O cool by pressing “O”.

8. Refill the main reservoir through the elbow at the back of the calorimeter.

The above procedure will only need to be done when the calorimeter is first filled with water after receiving it.

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.

CAUTION! Do not exceed the recommended energy release. Exceeding 8000 calories released per test could result in catastrophic failure.

CAUTION! Do not test samples containing metal using the 43AS Stainless Steel sample cups. Igniting samples with metal components could ignite the stainless steel sample cup and interior components of the vessel and damage the vessel. Samples containing metal can be tested with the 43A3 Fused Silica/Quartz crucibles.

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.

Quick Start6400 2 w w w . p a r r i n s t . c o m 17

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 OPERATING MODE key. Press the START Key. The calorimeter will now prompt the operator for sample ID number, Bomb ID num-ber, sample weight and spike weight in accor-dance with the instructions set into the operat-ing controls page.

8. The calorimeter will now take over and conduct the test. During the time it is establishing the ini-tial 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. Exam-ine the interior of the bomb for soot or other evidence of incomplete combustion. If such evidence is found, the test will have to be dis-carded.

If using the optional A1050DD Rinse Container Assembly:

11. Titrate the bomb washings with a standard sodium carbonate solution using methyl orange, red or purple indicator. A 0.0709N sodium car-bonate solution is recommended for this titra-tion 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.

3 Operation

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CHAPTER 3

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 cur-rent 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. Al-ways 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 val-ues 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 op-portunity for the user to confirm the specified action to minimize accidental disruptions to the program and/or stored data.

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. Abort. When a test is running the Start button changes to Abort. When pressed it will terminate the current test or pre-test.

5. 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 or printer.

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

7. This key appears in the Escape key loca-tion when the main menu is displayed. This key is used to shut down the calorimeter program before turning off the power.

Programming The program in the 6400 Calorimeter can be exten-sively 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, Operation6400 3 w w w . p a r r i n s t . c o m 19 techniques, combustion aids and short cuts appropri-ate 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 pre programmed with default settings. See Table 15-1 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 Set-tings, 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 experi-ences 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 configu-ration 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

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 stand-ing 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 pre-liminary tests indicate no abnormal behavior and the sample will not exceed the 8000 calorie limit.

CAUTION! Do not exceed the recommended energy release. Exceeding 8000 calories released per test could result in catastrophic failure.

Samples containing sulfur should contain no more than 50 mg of sulfur and liberate at least 5000 calories.

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

CAUTION! Do not test samples containing metal using the 43AS Stainless Steel sample cups.

Igniting samples with metal components could ignite the stainless steel sample cup and interior components of the vessel and damage the vessel.

Samples containing metal can be tested with the 43A3 Fused Silica/Quartz crucibles.

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 desir-able 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

P a r r I n s t r u m e n t C o m p a n y20 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.

Sample Types Because of the difference in combustion charac-teristics of the many different materials which may be burned in an oxygen bomb, it is difficult to give specific directions which will assure complete com-bustions 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 sup-port its own combustion regardless of the chilling effect of the adjacent metal parts.

The combustion must produce sufficient turbu-lence 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 par-ticles 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 ther-mal 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 rem-edied 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 addi-tives 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 pro-duced during the combustion process. The 1138CL is made from the halogen resistant Hastelloy G30™.

Hastelloy 30™ is an alloy rich in cobalt and molybde-num 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 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 hydro-statically tested to 3000 psi and the sample range is ~1g or 5000 – 8000 calories.

Explosives and High Energy Fuels

CAUTION! 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.

w w w . p a r r i n s t . c o m 21

Volatile Sample Holders Volatile samples are defined as one with an initial boiling point below 180 ºC. Volatile samples can be handled in a Parr 43AS Alloy Capsule which has a sturdy wall with a flat top rim. These holders can be sealed with a disc of plastic adhesive tape prepared by stretching tape across the top of the cup and trimming the excess with a sharp knife. 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 chlo-rine 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 3-1 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 determina-tion. 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 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 against the metal rim. Also cut and at-tach a small flag to the disc (see Figure 3-1).

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.

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 pres-sure 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 suit-able 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 re-duced 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 pos-sible damage to the bomb which might result from rapid combustion of the loose powder.

CAUTION! Do not exceed the recommended energy release. Exceeding 8000 calories released per test could result in catastrophic failure.

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/quartz, 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, P a r r I n s t r u m e n t C o m p a n y22 protective oxide film. This dull finish not only protects the capsule, but it also promotes combus-tion and makes it easier to burn the last traces of the sample. New capsules are heated in a muffle furnace at 500 ºC for 24 hours to develop this protec-tive coating uniformly on all surfaces. This treatment should be repeated after a capsule has been pol-ished 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 43A3 Fused Silica/Quartz Capsule is required.

CAUTION! Do not test samples containing metal using the 43AS Stainless Steel sample cups.

Igniting samples with metal components could ignite the stainless steel sample cup and interior components of the vessel and damage the vessel.

Samples containing metal can be tested with the 43A3 Fused Silica/Quartz crucibles.

When superior corrosion resistance is needed, the 43A5 Platinum Rhodium Capsule or 43A3 Fused Silica/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 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 heat-ing wire prior to attaching the cotton thread.

Four inches (10 cm) 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 (10 cm).

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.

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.

Figure 3-2 Cotton Thread Assembly w w w . p a r r i n s t . c o m 23

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

Figure 3-3 Bucket Fill Flow Diagram

BOMB WASH

A1589DD

RINSE

TANK

CLOSED

OPEN

BOMB FILL BOMB SEAL BOMB EXHAUST

WATER DRAIN WATER FILL COLD WATER

WATER TANK

PUMP TEMP

CONTROL

WATER

CHILLER

OXYGEN

INLET

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

2. The water fill solenoid opens and water is pumped from the internal tank into and through the bucket that surrounds the bomb. Overflow from the bucket is returned to the closed water tank.