Hanna Instruments HI 903 User manual

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HI 903
KARL FISCHER
VOLUMETRIC TITRATOR
Revision 1.0

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Dear customer,
Congratulations on choosing a Hanna Instruments Product.
This guide has been written for the HI 903 Karl Fischer Volumetric Titrator.
Please read this Quick Start Guide carefully before using the instrument. This guide will
provide you with the necessary information for the correct use of the instrument.
The purpose of this guide is to present a quick overview of setting up and using the
instrument.
For detailed information illustrating the extensive capabilities of your titrator, please refer to
the Instruction Manual.
© 2010 Hanna Instruments
All rights are reserved. Reproduction in whole or in part is prohibited without the written consent of the copyright
owner, Hanna Instruments Inc., 584 Park East Drive, Woonsocket, Rhode Island, 02895, USA.

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Contents
INTRODUCTION ..........................................................................................................3
SAFETY MEASURES.....................................................................................................4
TITRATOR CONNECTIONS .........................................................................................5
USER INTERFACE .........................................................................................................6
HOW TO SELECT YOUR LANGUAGE ............................................................................7
HOW TO USE THE CONTEXTUAL HELP .......................................................................7
METHODS ....................................................................................................................7
BEFORE PERFORMING THE FIRST TITRATION.........................................................8
HOW TO PERFORM THE FIRST TITRATION ..............................................................9

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INTRODUCTION
The HI 903 Karl Fischer volumetric titrator is extremely flexible, capable of performing a
wide variety of highly accurate and precise water content titration methods.
The HI 903 finds a titration endpoint using a polarized electrode and an advanced detection
algorithm. A constant flow of current is maintained between the two platinum pins of the
titrator’s electrode. When the solution in the titration vessel contains water, a relatively
large voltage is required to maintain the flow of current between the pins. As the titration
proceeds, the water in the sample is consumed by the titrant. At the end point, all of the
water has been reacted and the cell contains excess iodine. The presence of excess iodine
within the titration cell results in a reduction in the amount of voltage required to maintain
the constant current between the pins of the electrode. The endpoint detection algorithm
incorporated in the HI 903 analyzes both the electrode response to individual additions of
titrant and the shape of the entire titration curve in order to determine the endpoint of the
titration.
Titration reports and methods can be transferred to a PC via a USB interface, saved to a USB
flash drive or printed directly from the titrator. An external monitor and keyboard can be
attached for added convenience.
How can I find certain information?
1. This Quick Start Guide will help the user learn how to operate the titrator within
a short period of time. The first analysis will be performed with the aid of the
factory stored methods.
2. The Instruction Manual provides a complete description of the operating principles
(user interface, general options, methods, titration mode, maintenance, etc.).
3. The contextual Help screens contain detailed explanations about what kind of data
can be set or viewed in every displayed screen.
4. The Titration Theory booklet outlines the basic concepts of titration.

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SAFETY MEASURES
The following safety measures must be followed:
1. Always ensure that the power supply cable is connected to a grounded main power plug.
2. Never connect or disconnect the pump assemblies with the titrator turned on.
3. Verify that the burette and the attached tubing are as described in this guide.
4. Always check that the titrant, solvent and waste bottles, as well as the titration beaker are
properly assembled.
5. Always wipe up spills and splashes immediately.
6. Avoid the following environmental working conditions:
• Severe vibrations
• Direct sunlight
• Atmospheric relative humidity above 80% non-condensing
• Environment temperatures below 10
° C and above 40 ° C.
• Near heating or cooling sources
• Explosion hazards
7. Have the titrator serviced by qualified service personnel only.
8. Avoid inhalation of titrant/solvent vapors. Avoid contact with chemicals.

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TITRATOR CONNECTIONS
Front View
Rear View

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USER INTERFACE
Keypad
The titrators have their own keypad with 29 keys grouped in four categories, as follows:
Display
The titrators have a 5.7” graphical backlit color display. The Standby Mode screen is shown
below
with short explanations.
The user interface contains several screens. In each screen, many information fields are present
at the same time. The information is displayed in an easy-to-read manner, using different size
fonts.
Virtual option keys describe the function performed when the corresponding soft key is pressed.

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HOW TO SELECT YOUR LANGUAGE
To change the language, press from the main
screen. Highlight the
Language option and then press
. Using the and keys select the language
from the options listed in the
Set Language screen
and press .
Restart the titrator in order to apply the new language
setting.
HOW TO USE THE CONTEXTUAL HELP
Any information about the titrator can be easily accessed by pressing . The contextual
help can be accesed at any time and it provides useful information about the current screen.
METHODS
The HI 903 Karl Fischer titrator can store up to 100 methods: these include up to 90 stan-
dard methods.
Standard Methods
Each titrator is supplied with a customized package of standard methods. Standard method
packs are developed at Hanna Instruments laboratories to meet analysis requirements of
specific industries.
User-Defined Methods
User-defined methods allow the user to create and save their own methods. Each new
method is typically based on an existing method which is altered to suit a specific application.

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BEFORE PERFORMING THE FIRST TITRATION
Setup the Titrator
• Make sure that all of the titrator assemblies are properly installed (see Instruction
Manual,
Setup section).
• Make sure that the beaker system is properly sealed against atmospheric moisture
(the fittings and tubes are correctly mounted).
• The desiccant had been properly dried.
Obtaining the Reagents
• The reagents (titrant and solvent) have to be suitable to the analysis requirements
(see Instruction Manual,
Appendix 2 for list of preferred titrants and solvents).
Priming the Burette
• Remove the dispensing tube from titration beaker (unscrew the fitting and remove
the tube) and insert it in the waste bottle or separate waste container.
• From the
Idle screen press .
• Highlight the
Prime Burette option and then press .
• Enter the number of burette rinses. At least 3 rinses with the solution used for
titration are recommended (allowing air bubbles to be evacuated).
• Press to start.
• The message “Executing...” will be displayed.
Note: Make sure you have continuous liquid flow inside the burette. Do not use
Stop
Burette
during normal filling of the burette if you are not sure that air bubbles have been
completely evacuated. For accurate results, the aspiration tube, the dispensing tube
and the syringe must be free of air bubbles.
• Carefully wipe the end of the dispensing tube to remove excess titrant.
• Insert the dispensing tube in the corresponding hole of the titration beaker and
screw the fitting to seal the beaker.

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HOW TO PERFORM THE FIRST TITRATION
Method Selection
For this analysis we will use the HI8301EN Solvent with 5mg/ml 1-component
Titrant standard method
.
To select this method:
• Press from the
Idle screen. Use the and keys to highlight the HI8301EN
Solvent with 5mg/ml 1-component Titrant method.
• Press .
After accomplishing these operations, the method’s name will be displayed on the top line of
the
Idle screen.
Setting Method Parameters
To display the method parameters, press . The View/Modify Method screen will be
displayed.
Only certain parameters from the standard methods can be changed.
For this titration, only the KF titrant concentration value and the size of the solvent sample
need to be entered as in the screen shown below.
To accomplish this:
• Highlight
Titrant option from the View/Modify
Method
screen and then press .
• The
Karl Fischer Titrants screen will be displayed.
• Press .
• Highlight
“Standardized Titrant Concentration” and
press .
• Input the correct value, then press .
• Press three times to return to the
Idle screen.
Setup Titration Report
Users can select the information that is stored for each titration that is performed.
To obtain proper information at the end of the titration, perform the following operations:
• From the main screen, press and the
Data Parameters screen will be
displayed.

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• Highlight the Setup Titration Report option and press .
• Mark the fields to be included with the “*” symbol using the and keys and
press to toggle the selection.
• Press and then press to return to the main screen.
Fill Titration Beaker with Solvent
The titration beaker must be filled with 1-component up to the MIN marker (about 50 mL of
solvent):
• From the
Idle screen, press .
• Push and hold the FILL button located on the top of the air pump.
• Wait until the beaker is filled up to the MIN marker with solvent.
• Stop the air pump by pressing and then confirm the approximate amount of
solvent in the beaker.
Prepare the Solvent for Samples
Before beginning a titration, residual moisture inside the titration beaker and solvent must
be reacted:
• From the Idle screen, press . The titrator will enter Pre-Titration mode, start the
magnetic stirrer, and begin dosing titrant into the titration beaker. If no titrant can be
seen moving through the anti-diffusion tip after several doses, press and
verify that no titrant is leaking from the burette housing or from the dispensing tube
fittings.
• Once all residual moisture has been reacted (endpoint potential is reached), the titra-
tor will enter Drift Analysis mode (assuming Automatic Drift Entry is selected). The
titrator calculates the rate of atmospheric moisture seeping into the titration beaker for
the next minute and displays the result in the lower right corner of the display.
• If the Drift Rate is stable and the endpoint potential is maintained, the titrator will
enter Standby mode. The titrator continues to maintain the endpoint potential and
update the background drift rate.
Preparing and Introducing the Sample
Sample Mass Preparation
Measuring the sample size by mass using an analytical balance will give the most reproduc-

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ible results.
Solid Samples:
• Solid samples with larger pieces may need to be pulverized or ground in an analyti-
cal mill. These samples can be added with a weighing boat by removing the sample
port plug.
• Semisolid samples with non-homogeneous water content may need to be homog-
enized before addition. The sample can be added using a syringe without the needle
by removing the sample port plug.
Liquid Samples:
• Samples with low viscosity will be added using a syringe with needle (injection
through the septum).
Weigh the syringe before and after injection in order to increase precision.
Sample Volume Preparation
Liquid samples with low viscosity can be added by volume.
Samples should be added using a class A pipette.
Note: When adding samples using the weighing boat, pipette or syringe without needle, the
septum has to be removed. Therefore the adding operation should be performed quickly in
order to avoid the prolonged exposure of the beaker to atmospheric moisture.
Performing a Titration
• From the main screen press for analyzing a sample or for titrant stan-
dardization. You will be prompted to enter the analyte size. Add a prepared sample
according to a preparation method outlined above. Enter the analyte size and press
or . The titrator will start the analysis according to the selected method.
• At the end of the titration, the message “Titration Completed” will appear on the
titration status, together with the final concentration of the moisture in the sample,
the end point volume, and other relevant information. The titrator re-enters
Standby
mode (if active) in the background.

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Understanding the Displayed Information
During a titration, the following screen is displayed:
Viewing Graph During Titration
Press to display the real time titration graph.
The curve displayed is a plot of Electrode Potential vs. Titrant Volume.
A dashed horizontal line represents the user selected end point potential.
Titration Termination
The titration is terminated when the conditions of the Termination Criteria have been met.
The default Termination Criterion is a mV value, in which the titration is terminated after the
mV value remains below the end point potential for the selected stability time.
When the titration has ended, the titrator will display the final concentration of the moisture
together with the basic titration information.
To view the custom report or titration graph, press .
To view statistics of multiple analyses, press .
For titrant standardizations, press to update the active titrant with the displayed
standardization result.
When done, press to return to standby mode (if active).
Results
The results obtained from titration are stored in a re-
port file that can be displayed, transferred to a USB
storage device or a PC, or printed.
Viewing the last titration data
• Press (while no titration is being performed).
• The
Data Parameters screen will be displayed.
• From the
Data Parameters screen highlight the

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Review Last Titration Report option and press .
• The
Review Result screen will be displayed.
• Use the and keys to display information related to the last titration per-
formed.
See
titration report on page 15.
Printing the titration report
Connect a DOS / Windows compatible printer directly to the DB 25 connector (parallel port)
located on the back of the titrator.
Note: To connect the printer, please turn off the titrator and the printer.
Printing out the report:
• From the
Review Report screen, press .
• During the information transfer to the printer, the message “Printing” will be
displayed on the screen.
• Press to return to the
Data Parameters screen.
• Press again to return to the main screen.
Saving the data on a USB storage device
This feature allows saving the results of titrations or
drift logging sessions on a USB storage device.
• Insert the USB storage device into the USB
socket.
• From the
Idle screen, press . The Gen-
eral Options
screen will be displayed.
• Highlight the
Save Files to USB Storage De-
vice
option using the and keys.
• Press . The
List of Files on Titrator
screen will be displayed.
• Use the or keys to select the file type: “report files”.
• Press to transfer all available reports to USB storage device, or highlight the

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name of the report file to be transferred and press .
• Transferring a report file will automatically transfer the corresponding log file and
titration graph BMP file (if applicable).
• Press , to return to the
General Options screen.
• Press again, to return to the
Idle screen.
Titration report
While scrolling with the and keys, the fields below can be seen on the titrator
display or printed. The same information is available on the saved report file (KF_00003.rpt
in this example, with all report fields selected).
HI903 - Titration Report
Method Name: Moisture in Oil
Time & Date: 12:00 Jan 01, 2011
Titration ID: KF_00003
Company Name: Hanna Instruments
Operator Name: KF Technician
Electrode Name: Probe 1
Field 1: Any text
Field 2: Any text
Field 3: Any text
Titrator Software Version: v1.0
Base Board Software Version: v2.6
Pump Software Version: v1.4
Titrator Serial Number: 12345678
Analog Board Serial Number: 12345678
Pump Serial Number: 12345678
Analog Calibration Date: Aug 22, 2010
Method Parameters
Name: Moisture in Oil
Method Revision: 1.0
Type: Sample Analysis
Predispensing Rate None
Pre-Analysis Stir Time: 0 Sec
Stirring Speed: 900 RPM
Stirbar Type: Medium
Drift Entry: Automatic
Solvent: KF Solvent
Sample Parameters:
Sample Determ.: Normal
Sample Name: Oil
Sample Type: Mass
Sample Size: 0.5000 g
Titrant: KF Titrant
Titrant Type: One Component
Nominal Titrant Conc.: 2.0000 mg/mL
Stdz. Titrant Conc.: 2.0000 mg/mL
Date/Time: Jan 01, 2011 12:00
Titrant Age Reminder: 2d:00h:00m
Control Parameters:
Start Mode: Normal
Standby Mode: Enabled

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Standby Duration: 720 minutes
Imposed Current: 20 uA
Minimum Dose: 0.5000 uL
Maximum Dose: 30.0000 uL
Timed Increment: 1 second
End Point Value: 180.0 mV
Signal Averaging: 3 Readings
Flow Rate: 10.0 mL/min
Termination Parameters:
Maximum Duration: 3600 sec
Maximum Titrant Volume: 20.0000 mL
Term. Criterion: mV End Point
mV End Point: 4 sec
Result Unit: %
Nr Volume[ml] mV Time
0 0.0000 403.6 00:00:00
1 0.0000 403.5 00:00:01
2 0.0028 403.1 00:00:03
3 0.0078 402.3 00:00:05
4 0.0128 402.6 00:00:06
5 0.0178 403.0 00:00:08
6 0.0228 402.5 00:00:09
7 0.0278 402.4 00:00:11
8 0.0328 402.7 00:00:12
9 0.0378 402.5 00:00:14
10 0.0428 402.9 00:00:16
.
.
.
256 0.9904 169.7 00:06:45
257 0.9904 177.4 00:06:47
258 0.9904 173.7 00:06:48
259 0.9904 171.1 00:06:50
260 0.9904 173.4 00:06:52
261 0.9904 181.1 00:06:53
262 0.9904 175.5 00:06:55
263 0.9904 178.2 00:06:56
264 0.9904 177.6 00:06:58
Titration Results
Method Name: Moisture in Oil
Time & Date: 12:00 Jan 01, 2011
Sample Size: 0.5291 g
Titrant Conc.: 2.0000 mg/mL
Drift Value: 1.0 ug/min
End Point Volume: 0.9904 mL
Result: 0.3730 %
Titration Duration: 06:58 [mm:ss]
Estimated Cell Volume: 50.8 mL
Titration went to Completion
Operator Name: Any text
Analyst Signature: ____________________

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QS 903
02/11

1
INSTRUCTION MANUAL
HI 903
KARL FISCHER
VOLUMETRIC TITRATOR
Revision 1.00

2
Dear customer,
Congratulations on choosing a Hanna Instruments product.
Please read this instruction manual carefully before using the instrument. This manual will
provide you with the necessary information for the correct use of the instrument.
© 2010 Hanna Instruments
All rights are reserved. Reproduction in whole or in part is prohibited without the written consent of the copyright
owner, Hanna Instruments Inc., 584 Park East Drive, Woonsocket, Rhode Island 02895, USA.