Parr Instrument 6400 Bedienungsanleitung

587M

6400

Automatic Isoperibol Calorimeter

Operating Instruction Manual

For models produced after October 2010

www.parrinst.com

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 19

Default Settings 19

Sample Preparation 19

Test Process 22

Closing the bomb 22

Cool/Rinse 26

Drain

Fill Cycle 23

Pre-Period 24

Bomb Firing 25

Post-Period 25

Chapter 4 28

Menu Descriptions 28

Main Menu 28

Calorimeter Operation Menu 28

Temperature vs. 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 39

Auto Sample ID Controls 39

Moisture Data Entry Controls 40

Preweigh Sample ID Controls 40

Reporting Controls Menu 40

Communication Controls Menu 41

Balance Port Communications 41

Balance Port Settings 42

File Management Menu 43

Run Data File Manager 43

Diagnostics Menu 44

Data Logger Controls 44

Data Log Items 45

User Deﬁned Buttons 45

I/O Diagnostics:

Parr Instrument Company

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

Samba Server Feature (Optional) 59

Bar Code Port 66

Chapter 9 68

Memory Management 68

Clearing Memory 68

Removable SD Memory 68

Chapter 10 70

Maintenance 70

Inspection of Critical Sealing Surfaces 70

Bomb 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

1138 Parts Diagram Key 83

Chapter 15 104

Tables 104

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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 14-1

1138 Parts Diagram 82

Figure 14-2

6400 Cutaway Right 84

Figure 14-3

6400 Cutaway Left 85

Figure 14-4

6400 Cover Open 86

Figure 14-5

A1250DD2 Control Schematic 87

Figure 14-6

A1251DD Oxygen Solenoid Assembly 88

Figure 14-7

A1447DD Water Solenoid Assembly 88

Figure 14-8

A1456DD Rinse Valve Assembly 89

Figure 14-9

6400 Internal Plumbing Diagram 90

Figure 14-10

6400 Water Tank and Jacket Cooling Solenoid 91

Tables

Table 6-1

Calorimeter Control Limit Values in J/g When Benzoic

Acid is Used as a Test Sample 49

Table 6-2

Calorimeter Control Limit 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 14-11

A1455DD Propeller Assembly 92

Figure 14-12

A1448DD Temperature Control Assembly 92

Figure 14-13

A1268DD Stirrer Motor and Mount 93

Figure 14-14

6400 Bucket Assembly 94

Figure 14-15

6400 Air Can Assembly, Cutaway Left 95

Figure 14-16

6400 Air Can Assembly, Cutaway Front 96

Figure 14-17

A1450DD Bomb Head Assembly, View 1 97

Figure 14-18

A1450DD Bomb Head Assembly, View 2 98

Figure 14-19

A1050DD Rinse Collection Assembly 99

Figure 14-20

Wiring Diagram 100

Figure 14-21

Wiring Diagram 101

Figure 14-22

Fuse Diagram 102

Preface

Parr Instrument Company

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 InternationalTable 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.

Customer Service

Questions concerning the installation or operation of this instrument

can be answered by the Parr Customer Service Department:

1-309-762-7716 • 1-800-872-7720 • Fax: 1-309-762-9453

E-mail: par[email protected] • http://www.parrinst.com

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.

Preface

6400

www.parrinst.com 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

Parr Instrument Company

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 and 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.

www.parrinst.com 7

Notes

6400

1Installation

Parr Instrument Company

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 SwagelokTube Fittings are used, the instruc-

tions for installation are:

1. Simply insert the tubing into the SwagelokTube

Fitting. Make sure that the tubing rests ﬁrmly

on 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 ttings, tight-

en the Swagelok nut 3/4 turns from nger-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.

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