Hanna Instruments | HI933 | Owner Manual | Hanna Instruments HI933 Owner Manual

Hanna Instruments HI933 Owner Manual
HI933
KARL FISCHER
VOLUMETRIC TITRATOR
Dear
Customer,
Thank you for choosing a Hanna Instruments product.
Please read this instruction manual carefully before using this instrument. This manual will provide
you with the necessary information for the correct use of this instrument, as well as a precise idea of
its versatility.
If you need additional technical information, do not hesitate to e-mail us at tech@hannainst.com or view
our worldwide contact list for a Hanna Instruments representative near you at www.hannainst.com.
© 2019 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.,
Woonsocket, Rhode Island, 02895, USA.
INTRODUCTION
The HI933 is an automatic volumetric Karl Fischer titrator with high accuracy, great flexibility and repeatability. It is
designed to perform titrations for a variety of sample types/matrices, allowing the user to obtain both good results and
high-speed analysis.
The main attributes of the HI933 titrator are:
• Small footprint, requires minimal bench space
• Casing made with strong, chemically resistant plastic
• Powerful built-in algorithms for termination criteria based on fixed mV endpoint or absolute/relative drift
• Titrant standardization and sample analysis averaging
• Minimized water vapor entry with the Sealed Solvent System
• Balance interface for automatic weighing
• Support for 100 titration methods
• User-customizable reports
• Clearly displayed warning and error messages
This manual provides information regarding installation and functionality of the titrator and refined operation suggestions.
Before using the titrator, it is recommended you become familiar with its various features and functionality.
This manual is divided into four parts:
PART 1: QUICK START GUIDE
Helps the user quickly setup and operate HI933 Karl Fisher titrator. It covers basic connections, user interface and how
to run a titration.
PART 2: INSTRUCTION MANUAL
Provides a comprehensive description of the operating principles user interface, general options, methods, titration
mode, optimization, maintenance, etc.
PART 3: APPLICATIONS
Contains complete instructions for commonly-used analyses. Additional methods and method packs are available;
contact your local Hanna Instruments office for more details.
PART 4: TITRATION THEORY
Outlines the principles of operation of the titrator. It covers the chemistry of titrations, titration types and result
calculations.
III
TABLE OF CONTENTS
PART 1: QUICK START GUIDE
1. SAFETY MEASURES.......................................................................................................................................................... 1-2
2. TITRATOR CONNECTIONS.................................................................................................................................................. 1-3
2.1. FRONT VIEW......................................................................................................................................................... 1-3
2.2. REAR VIEW........................................................................................................................................................... 1-3
3. USER INTERFACE............................................................................................................................................................. 1-4
3.1. KEYPAD................................................................................................................................................................ 1-4
3.2. DISPLAY............................................................................................................................................................... 1-4
4. LANGUAGE...................................................................................................................................................................... 1-5
5. CONTEXTUAL HELP........................................................................................................................................................... 1-5
6. METHODS....................................................................................................................................................................... 1-5
6.1. STANDARD METHODS............................................................................................................................................ 1-5
6.2. USER-DEFINED METHODS...................................................................................................................................... 1-5
7. PREPARATION.................................................................................................................................................................. 1-6
7.1. SETTING UP THE TITRATOR..................................................................................................................................... 1-6
7.2. OBTAINING THE REAGENTS.................................................................................................................................... 1-6
7.3. PRIMING THE BURETTE.......................................................................................................................................... 1-6
8. THE FIRST TITRATION ...................................................................................................................................................... 1-7
8.1. METHOD SELECTION.............................................................................................................................................. 1-7
8.2. SETTING METHOD PARAMETERS............................................................................................................................. 1-7
8.3. SETTING UP TITRATION REPORT............................................................................................................................. 1-7
8.4. FILLING TITRATION BEAKER WITH SOLVENT............................................................................................................. 1-8
8.5. PREPARING THE SOLVENT FOR SAMPLES................................................................................................................. 1-8
8.6. PREPARING AND INTRODUCING THE SAMPLE........................................................................................................... 1-8
8.7. PERFORMING A TITRATION..................................................................................................................................... 1-9
8.8. UNDERSTANDING THE DISPLAYED INFORMATION.................................................................................................... 1-9
8.9. VIEWING GRAPH DURING TITRATION.................................................................................................................... 1-10
8.10. TITRATION TERMINATION................................................................................................................................... 1-10
8.11. RESULTS.......................................................................................................................................................... 1-11
8.12. VIEWING THE LAST TITRATION DATA................................................................................................................... 1-11
8.13. PRINTING THE TITRATION REPORT...................................................................................................................... 1-11
8.14. SAVING DATA TO USB STORAGE DEVICE.............................................................................................................. 1-12
8.15. TITRATION REPORT............................................................................................................................................ 1-13
PART 2: INSTRUCTION MANUAL
1. SETUP............................................................................................................................................................................. 2-2
1.1. UNPACKING.......................................................................................................................................................... 2-2
1.2. SAFETY MEASURES................................................................................................................................................ 2-3
1.3. TECHNICAL SPECIFICATIONS................................................................................................................................... 2-4
1.4. INSTALLATION....................................................................................................................................................... 2-5
2. USER INTERFACE........................................................................................................................................................... 2-13
2.1. START UP........................................................................................................................................................... 2-13
2.2. KEYPAD.............................................................................................................................................................. 2-13
2.3. DISPLAY............................................................................................................................................................. 2-15
2.4. MENU NAVIGATION............................................................................................................................................. 2-16
3. GENERAL OPTIONS......................................................................................................................................................... 2-18
3.1. SAVE FILES TO USB STORAGE DEVICE................................................................................................................... 2-18
3.2. RESTORE FILES FROM USB STORAGE DEVICE......................................................................................................... 2-19
3.3. STANDBY MODE.................................................................................................................................................. 2-20
IV
4.
5.
6.
7.
8.
9.
3.4. STANDBY DURATION........................................................................................................................................... 2-20
3.5. TITRANT DATABASE............................................................................................................................................. 2-21
3.6. STANDARD DATABASE.......................................................................................................................................... 2-21
3.7. ESTIMATED CELL VOLUME.................................................................................................................................... 2-22
3.8. USB LINK WITH PC.............................................................................................................................................. 2-22
3.9. SETUP BALANCE INTERFACE................................................................................................................................. 2-23
3.10. STIRRER........................................................................................................................................................... 2-24
3.11. PRINTER MODE................................................................................................................................................. 2-24
3.12. DATE AND TIME SETTING................................................................................................................................... 2-25
3.13. DISPLAY SETTINGS............................................................................................................................................ 2-25
3.14. BEEPER............................................................................................................................................................ 2-26
3.15. LANGUAGE........................................................................................................................................................ 2-26
3.16. CALIBRATION CHECK.......................................................................................................................................... 2-27
3.17. RESET TO DEFAULT SETTINGS............................................................................................................................. 2-27
3.18. OPTIMIZE MEMORY SPACE................................................................................................................................. 2-28
3.19. UPDATE SOFTWARE........................................................................................................................................... 2-28
TITRATION METHODS..................................................................................................................................................... 2-29
4.1. SELECTING METHODS.......................................................................................................................................... 2-29
4.2. STANDARD METHODS.......................................................................................................................................... 2-29
4.3. USER METHODS.................................................................................................................................................. 2-31
4.4. VIEWING / MODIFYING METHOD.......................................................................................................................... 2-32
4.5. METHOD OPTIONS............................................................................................................................................... 2-33
4.6. PRINTING........................................................................................................................................................... 2-58
TITRATION MODE........................................................................................................................................................... 2-59
5.1. IDLE................................................................................................................................................................... 2-59
5.2. PRE-TITRATION................................................................................................................................................... 2-60
5.3. DRIFT ANALYSIS (AUTOMATIC DETERMINATION ENTRY ONLY)................................................................................. 2-60
5.4. STANDBY............................................................................................................................................................ 2-61
5.5. SAMPLE ANALYSIS............................................................................................................................................... 2-62
5.6. TITRANT STANDARDIZATION................................................................................................................................. 2-67
AUXILIARY FUNCTIONS................................................................................................................................................... 2-70
6.1. AIR PUMP........................................................................................................................................................... 2-70
6.2. BURETTE............................................................................................................................................................ 2-71
6.3. STIRRER............................................................................................................................................................. 2-73
6.4. RESULTS............................................................................................................................................................ 2-73
MAINTENANCE AND PERIPHERALS................................................................................................................................... 2-77
7.1. BURETTE MAINTENANCE...................................................................................................................................... 2-77
7.2. PROBE MAINTENANCE......................................................................................................................................... 2-80
7.3. PERIPHERALS..................................................................................................................................................... 2-80
METHOD OPTIMIZATION................................................................................................................................................. 2-83
8.1. TITRATION SETTINGS........................................................................................................................................... 2-83
8.2. CONTROL PARAMETERS........................................................................................................................................ 2-83
8.3. THE SAMPLE....................................................................................................................................................... 2-87
8.4. KARL FISCHER REAGENT SYSTEM.......................................................................................................................... 2-92
ACCESSORIES................................................................................................................................................................ 2-95
9.1. TITRANTS........................................................................................................................................................... 2-95
9.2. SOLVENTS.......................................................................................................................................................... 2-95
9.3. STANDARDS........................................................................................................................................................ 2-96
9.4. TITRATOR COMPONENTS...................................................................................................................................... 2-97
V
PART 3: APPLICATIONS
HI8001EN 5.0 mg/mL TITRANT STANDARDIZATION WITH WATER STANDARD............................................................................. 3-2
HI8002EN 2.0 mg/mL TITRANT STANDARDIZATION WITH WATER STANDARD............................................................................. 3-4
HI8003EN 1.0 mg/mL TITRANT STANDARDIZATION WITH WATER STANDARD............................................................................. 3-6
HI8011EN 5.0 mg/mL TITRANT STANDARDIZATION WITH DISODIUM TARTRATE......................................................................... 3-8
HI8101EN MOISTURE DETERMINATION IN DAIRY CREAM....................................................................................................... 3-10
HI8102EN MOISTURE DETERMINATION IN MILK.................................................................................................................... 3-12
HI8103EN MOISTURE DETERMINATION IN HONEY................................................................................................................. 3-14
HI8104EN SURFACE MOISTURE DETERMINATION ON WHITE SUGAR....................................................................................... 3-16
HI8105EN MOISTURE DETERMINATION IN COOKING OIL........................................................................................................ 3-18
HI8106EN MOISTURE DETERMINATION IN BUTTER................................................................................................................ 3-20
HI8107EN MOISTURE DETERMINATION IN MARGARINE......................................................................................................... 3-22
HI8108EN MOISTURE DETERMINATION IN MAYONNAISE....................................................................................................... 3-24
HI8201EN MOISTURE DETERMINATION IN SHAMPOO............................................................................................................ 3-26
HI8202EN MOISTURE DETERMINATION IN HAND CREAM....................................................................................................... 3-28
HI8301EN MOISTURE DETERMINATION IN SOLVENT WITH 5 mg/mL TITRANT (ONE-COMP.)...................................................... 3-30
PART 4: TITRATION THEORY
1. TITRATION THEORY.......................................................................................................................................................... 4-2
1.1. INTRODUCTION TO TITRATIONS.............................................................................................................................. 4-2
1.2. USES OF TITRATIONS............................................................................................................................................ 4-2
1.3. ADVANTAGES AND DISADVANTAGES OF TITRATIONS................................................................................................. 4-2
2. TYPES OF TITRATIONS...................................................................................................................................................... 4-3
2.1. TITRATIONS ACCORDING TO THE MEASUREMENT METHOD........................................................................................ 4-3
2.2. TITRATIONS ACCORDING TO THE REACTION TYPE...................................................................................................... 4-4
2.3. TITRATIONS ACCORDING TO THE TITRATION SEQUENCE.......................................................................................... 4-11
3. TITRATION PROCEDURE.................................................................................................................................................. 4-12
3.1. MANUAL TITRATION............................................................................................................................................. 4-12
3.2. AUTOMATIC TITRATION ....................................................................................................................................... 4-12
4. TITRATION RESULTS....................................................................................................................................................... 4-14
4.1. ACCURACY.......................................................................................................................................................... 4-14
4.2. REPEATABILITY.................................................................................................................................................... 4-14
4.3. SOURCES OF ERROR........................................................................................................................................... 4-14
5. CALCULATIONS.............................................................................................................................................................. 4-16
5.1. EQUATIONS USED IN VOLUMETRIC KARL FISCHER TITRATIONS............................................................................... 4-16
5.2. EQUATIONS USED IN TITRATIONS......................................................................................................................... 4-18
6. GLOSSARY..................................................................................................................................................................... 4-21
VI
PART 1:
QUICK START GUIDE
QUICK START GUIDE
1
QUICK START GUIDE
1
1-2
1. SAFETY MEASURES
The following safety measures must be followed:
1) Never connect or disconnect the pump assembly or other peripheral with the titrator turned on.
2) Verify that the burette and the attached tubing are assembled correctly.
3) Always check that the titrant, solvent and waste bottles, as well as the titration beaker are properly assembled.
4) Always wipe up spills and splashes immediately.
5) 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
• Explosion hazards
• Near heating or cooling sources
6) Have the titrator serviced by qualified service personnel only.
7) Avoid inhalation of titrant/solvent vapors. Avoid contact with chemicals.
1
2. TITRATOR CONNECTIONS
2.1. FRONT VIEW
Titrant Bottle
Solvent Bottle
Titrant Bottle
Assembly
Waste Bottle
Assembly
Dispensing Tube
QUICK START GUIDE
Solvent Bottle
Assembly
Aspiration
Tube
Waste Bottle
Burette Assembly
Air Pump and
Magnetic Stirrer
Beaker Assembly
USB
2.2. REAR VIEW
Beaker Desiccant
Fittings
Locking Screws
On/Off Button
Balance Interface Connector
External
Magnetic Stirrer
KF Electrode
Input
PC Interface
Printer Connector
PC Keyboard
Connector
Power Adapter
Connector
1-3
1
3. USER INTERFACE
QUICK START GUIDE
3.1. KEYPAD
The titrator’s keypad has 27 keys grouped in five categories, as follows:
Numeric
Keys
Function
Keys
Arrow
Keys
Option Keys
Enter Key
3.2. DISPLAY
The titrator has a 5.7” graphical backlit color display. The Standby Mode screen is shown below with short explanations.
Process status icon
Process status
Time and Date
Method name
Process stage
Burette icon
Last dose volume
Stirrer speed
Reminders or Messages
Pre-titration/Titration volume
mV value
Drift value
Virtual option keys
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.
Virtual option keys describe the function performed when the corresponding soft key is pressed.
1-4
1
4. LANGUAGE
and
keys,
QUICK START GUIDE
To change the language, press
from the main screen. Highlight Language option. Using the
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.
5. CONTEXTUAL HELP
Information about the titrator can be easily accessed by pressing
and it provides useful information about the current screen.
. The contextual help can be accessed at any time
6. METHODS
The HI933 Karl Fischer titrator can store up to 100 methods (standard and user defined).
6.1. STANDARD METHODS
Each titrator is supplied with a customized package of standard methods. Standard method packs are developed at
Hanna Instruments to meet analysis requirements of specific industries (e.g.: food, cosmetics, dairy, etc.).
6.2. USER-DEFINED METHODS
User-defined methods allow the user to create and save their own methods. Each new method is based on an existing
method which is altered to suit a specific application.
1-5
1
7. PREPARATION
QUICK START GUIDE
7.1. SETTING UP THE TITRATOR
• Make sure that all of the titrator assemblies are properly installed (see Setup section).
• Make sure that the beaker system is properly sealed against atmospheric moisture (the fittings and tubes are
correctly mounted).
• The desiccant has been properly dried.
7.2. OBTAINING THE REAGENTS
• The reagents (titrant and solvent) have to be suitable to the analysis requirements (see Accessories section for
list of preferred titrants and solvents).
7.3. 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 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
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.
1-6
1
8. THE FIRST TITRATION
8.1. METHOD SELECTION
8.2. SETTING METHOD PARAMETERS
QUICK START GUIDE
For this analysis we will use the HI8301EN Solvent w/ 5mg/ml 1-comp standard method.
To select this method:
• Press
from the Idle screen. Use the
and
keys to highlight HI8301EN Solvent w/ 5mg/ml
1-comp method.
• Press
.
The method’s name will be displayed on the top line of the Idle screen.
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 Titrant Database screen will be displayed.
• Highlight KF Titrant and press
.
• Highlight Standardized Titrant Concentration and press
.
• Input the correct value, then press
.
• Press
three times to return to the Idle screen.
8.3. SETTING UP TITRATION REPORT
Users can select the information that is stored for each titration.
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.
• Highlight Setup Titration Report option and press
.
• Mark the fields to be included with the * symbol using the and keys, and press
selection.
• Press
and then press
to return to the main screen.
to toggle the
1-7
QUICK START GUIDE
1
8.4. FILLING TITRATION BEAKER WITH SOLVENT
The titration beaker must be filled with solvent up to the minimum (MIN) mark (about 50 mL of solvent):
• From the Idle screen, press
.
• Press
.
• Wait until the beaker is filled up to the minimum (MIN) mark with solvent.
• Stop the air pump by pressing
• Press
then enter the approximate amount of solvent in the beaker. Press
to confirm.
8.5. PREPARING 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 and begin dosing titrant into the
titration beaker. If no titrant can be seen moving through the anti-diffusion tip after several doses, press
or
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 titrator will enter Drift Analysis
mode (Automatic Drift Entry only). 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.
8.6. PREPARING AND INTRODUCING THE SAMPLE
Measuring the sample size by mass and using an analytical balance will give the most reproducible results.
• Prepare 50 mL of sample by mixing equal parts of dry chloroform and dry methanol.
• Fill the syringe and needle with the sample.
• Weigh the syringe, needle and sample.
• Press
. You will be prompted to enter the sample size.
• Dispense 0.750 g to 1.000 g of solvent into the titration vessel through the septum using the needle.
• Remove the needle from the titration vessel and weigh the syringe again in order to determine the added sample
mass (by difference of the two measurements.)
• Use the numeric keypad to enter the exact weight and press
to start the analysis.
1-8
8.7. PERFORMING A TITRATION
QUICK START GUIDE
• Add a prepared sample according to one of the preparation methods outlined above. Enter the analyte size and
press
. 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 in the background.
1
8.8. UNDERSTANDING THE DISPLAYED INFORMATION
During a titration, the following screen is displayed:
1-9
QUICK START GUIDE
1
8.9. 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.
Note: For fresh solvents, especially one-component solvents, the first few titration graphs may look very noisy. This is
because the reaction with the titrant is sluggish if there is a low amount of excess Karl Fischer reagent (sulfur dioxide
and base) in the titration vessel. After several titrations, the reaction speed and graph should improve.
8.10. 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).
1-10
8.11. RESULTS
QUICK START GUIDE
The results obtained from titration are stored in a report file that can be displayed, transferred to a USB storage device
or a PC, or printed.
1
8.12. VIEWING THE LAST TITRATION DATA
• From the main screen, press
. The Data Parameters screen will be displayed.
• From the Data Parameters screen highlight Review Last Report option and press
. The Review Result
screen will be displayed.
• Use the
and
keys to display information related to the last titration performed.
See Titration Report on next page.
8.13. PRINTING THE TITRATION REPORT
Connect a DOS / Windows-compatible parallel printer directly to the DB 25 pin connector located on the back of the
titrator.
Note: Prior to connecting the printer, ensure that the titrator and the printer have been turned off.
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.
1-11
1
8.14. SAVING DATA TO USB STORAGE DEVICE
QUICK START GUIDE
Note: The USB Storage Device has to be formatted FAT or FAT32.
This feature allows saving the results of titrations or drift logging sessions on a USB storage device.
• From the main screen, press
, the General Options screen will be displayed.
• Highlight Save Files to USB Storage Device option using the and keys.
• Insert the USB storage device into the USB socket.
• Press
, the List of Files on Titrator screen will be displayed.
• Use the and keys to select the report files.
• Press
to transfer all available reports to the USB storage device, or highlight the 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 main screen.
1-12
8.15. TITRATION REPORT
HI933 - Titration Report
Method Name:
Time & Date:
Titration ID:
Nr
0
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
Moisture in brake fluid
16:59 Dec 19, 2018
KF_00010
Volume[ml]
0.0000
0.3261
0.3276
0.3306
0.3366
0.3486
0.3726
0.4126
0.4526
0.4926
0.5326
0.5726
0.6126
0.6526
0.6926
0.7326
0.7726
0.8126
0.8526
0.8926
0.9326
0.9726
1.0126
1.0526
1.0926
1.1326
1.1726
1.2126
1.2526
1.2926
1.3300
1.3671
1.3856
1.3949
1.3995
1.4017
1.4062
1.4062
1.4077
mV
685.5
685.0
684.9
684.1
683.7
682.7
681.7
678.0
675.5
673.0
671.6
669.6
667.6
666.7
665.9
665.0
659.2
654.9
654.1
649.6
646.7
635.8
633.9
622.4
615.2
587.8
584.5
550.1
524.0
452.3
405.6
290.6
227.5
197.5
183.4
187.7
177.3
184.0
178.8
Time
00:00:00
00:00:02
00:00:04
00:00:06
00:00:08
00:00:10
00:00:12
00:00:15
00:00:17
00:00:19
00:00:21
00:00:23
00:00:25
00:00:27
00:00:29
00:00:31
00:00:33
00:00:35
00:00:37
00:00:39
00:00:41
00:00:43
00:00:45
00:00:47
00:00:49
00:00:51
00:00:53
00:00:55
00:00:57
00:00:59
00:01:01
00:01:03
00:01:05
00:01:07
00:01:09
00:01:11
00:01:14
00:01:16
00:01:18
QUICK START GUIDE
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).
1
1-13
QUICK START GUIDE
1
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65
66
67
68
69
70
1.4077
1.4077
1.4077
1.4077
1.4077
1.4077
1.4092
1.4107
1.4107
1.4107
1.4107
1.4122
1.4122
1.4122
1.4122
1.4122
1.4137
1.4167
1.4167
1.4167
1.4167
1.4167
1.4167
1.4167
1.4182
1.4182
1.4182
1.4197
1.4197
1.4197
1.4212
1.4212
174.7
180.2
174.7
175.8
179.3
186.2
182.1
177.5
174.2
177.0
183.3
174.0
175.3
175.9
181.6
181.9
185.7
174.6
170.3
173.4
174.6
174.5
177.2
188.1
179.7
176.2
185.7
179.6
175.7
184.0
169.9
178.2
00:01:20
00:01:22
00:01:24
00:01:26
00:01:28
00:01:30
00:01:32
00:01:34
00:01:36
00:01:38
00:01:40
00:01:42
00:01:44
00:01:46
00:01:48
00:01:50
00:01:52
00:01:54
00:01:56
00:01:58
00:02:00
00:02:02
00:02:04
00:02:06
00:02:08
00:02:10
00:02:12
00:02:14
00:02:17
00:02:19
00:02:21
00:02:23
Titration Results
Method Name:
Moisture in brake fluid
Time & Date
16:59 Dec 19, 2018
Sample Size:
0.6585 g
Std. Titrant Conc.:
1.1608 mg/mL
Drift Value:
15.2 µg/min
End Point Volume:
1.421 mL
Result:
0.2429 %
Titration Duration:
03:18 [mm:ss]
Estimated Cell Volume:
69.9 mL
Titration went to Completion
Operator Name:
Analyst Signature: _____________________
1-14
PART 2:
INSTRUCTION MANUAL
INSTRUCTION MANUAL
2

2
1. SETUP
SETUP
INSTRUCTION MANUAL
1.1. UNPACKING
2-2
Remove the titrator and accessories from the packaging and examine it carefully to make sure that no damage has
occurred during shipping. Notify your nearest Hanna Service Center if damage is observed.
Each HI933 titrator is supplied with:
ITEM
QUANTITY
Titrator..................................................................................................................................................... 1 pc
Dosing Pump Assembly.............................................................................................................................. 1 pc
Burette Assembly....................................................................................................................................... 1 pc
• Burette (with 5 mL syringe)
• Aspiration Tube with Fitting and Protection Tube
• Dispensing Tube with Fitting and Protection Tube
• Tube Locks
• Tool for Burette Cap Removal
• Light Protection Screen
Air Pump and Magnetic Stirrer Assembly...................................................................................................... 1 pc
Beaker Assembly....................................................................................................................................... 1 pc
• Glass Beaker
• Anti-diffusion Glass Dispensing Tip
• Beaker Ring
• Beaker Cap
• Stir Bar
• Desiccant
• Desiccant Cartridge
• Fittings
• O-rings
Beaker Support......................................................................................................................................... 1 pc
Pump Locking Screws with Plastic Head....................................................................................................... 2 pcs
Titrant Bottle Assembly.............................................................................................................................. 1 pc
• Bottle Cap
• Desiccant
• Desiccant Cartridge
• Fittings
• O-rings
Solvent Bottle Assembly............................................................................................................................. 1 pc
• Bottle Cap
• Desiccant
• Desiccant Cartridge
• Fittings
• O-rings
• Tubes (Silicone and PTFE Tubing)
2
INSTRUCTION MANUAL
Waste Bottle Assembly............................................................................................................................... 1 pc
• Bottle Cap
• Desiccant
• Desiccant Cartridge
• Fittings
• O-rings
• Tubes (Silicone and PTFE Tubing)
Karl Fischer Dual Platinum Pin Electrode...................................................................................................... 1 pc
Calibration Key.......................................................................................................................................... 1 pc
Power Supply............................................................................................................................................ 1 pc
USB Cable................................................................................................................................................ 1 pc
Instruction Manual.................................................................................................................................... 1 pc
USB Storage Device................................................................................................................................... 1 pc
Quality Certificate...................................................................................................................................... 1 pc
ISO 8655 Burette Compliance Report.......................................................................................................... 1 pc
See Accessories section for pictures.
If any of the items are missing or damaged, please contact your sales representative.
Note: Save all packing materials until you are sure that the instrument functions correctly. Any damaged or defective
items must be returned in their original packing materials together with the supplied accessories.
1.2. SAFETY MEASURES
SETUP
The following safety measures must be followed:
1) Never connect or disconnect the dosing pump or air pump and magnetic stirrer assemblies with the titrator turned
on.
2) Verify that the burette and the attached tubing are assembled correctly (see Maintenance, Peripherals, Burette
Maintenance for more details).
3) Always check that the titrant, solvent, waste bottles and the titration beaker are properly assembled.
4) Always wipe up spills and splashes immediately.
5) 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
• Explosion hazards
6) Have the titrator serviced only by qualified service personnel.
2-3
INSTRUCTION MANUAL
2
1.3. TECHNICAL SPECIFICATIONS
Measurement
Determination
SETUP
Titration
System
Electrode
Stirrer
Storage
Peripheral
Devices
2-4
Range
Resolution
Result Units
Sample Type
100 ppm to 100%
1 ppm to 0.0001%
%, ppm, mg/g, μg/g, mg, μg, mg/mL, μg/mL, mg/pc, μg/pc
Liquid or Solid
Pre-Titration Conditioning
Automatic
Background Drift Correction
Endpoint Criteria
Dosing
Result Statistics
Dosing Pump Resolution
Dosing Pump Accuracy
Syringe
Valve
Tubing
Dispensing Tip
Titration Vessel
Solvent Handing System
Type
Connection
Polarization Current
Voltage Range
Voltage Resolution
Accuracy
Type
Speed
Resolution
Methods
Reports
PC Connection
USB flash drive
Analytical Balance
Printer
External PC Keyboard
Automatic or User Selectable Value
Fixed mV persistence, Relative drift stop or Absolute drift stop
Dynamic with optional pre-dispensing
Mean, Standard Deviation
1/40000 of the burette volume (0.125 μL per dose)
± 0.1% of full burette volume
5 mL precision ground with PTFE plunger
Motor-driven 3-way, PTFE liquid contact material
PTFE with light block and thermal jacketing
Glass, fixed position anti-diffusion
Conical with operating volume between 50-150 mL
Sealed system, integrated diaphragm air pump
Dual platinum pin, polarization electrode
BNC
1, 2, 5, 10, 15, 20, 30 or 40 μA
2 mV to 1000 mV
0.1 mV
± 0.1%
Magnetic, electronic regulated, digital stirrer
200 to 2000 RPM
100 RPM
Up to 100 (standard and user defined) methods
Up to 100 complete titration reports and drift rate reports
1 x USB Standard B
1 x USB Standard A
1 x DB-9 Socket
1 x DB-25 Socket
1 x 6-pin Mini DIN
5.7" graphical color display with backlight
English, Portuguese, Spanish, French
100-240 Vac, 50/60 Hz
0.5 Amps
ABS, PC and Stainless Steel
Polyester
315 x 205 x 375 mm (12.4 x 8.1 x 14.8 ")
approx. 4.3 kg (9.5 lbs.) with 1 pump, stirrer and sensors
10 to 40 °C (50 to 104 °F); up to 80 % RH
-20 to 70 °C (-4 to 158 °F); up to 95 % RH
2
INSTRUCTION MANUAL
Additional
Specifications
Display
Languages
Power Supply
Power Draw
Enclosure Material
Keypad
Dimensions
Weight
Operating Environment
Storage Environment
1.4. INSTALLATION
1.4.1. TITRATOR RIGHT VIEW
Solvent Bottle
Assembly
Aspiration
Tube
Titrant Bottle
Solvent Bottle
Titrant Bottle
Assembly
Waste Bottle
Assembly
Waste Bottle
SETUP
Dispensing Tube
Burette Assembly
Air Pump and
Magnetic Stirrer
Beaker Assembly
USB
2-5
2
1.4.2. TITRATOR REAR VIEW
INSTRUCTION MANUAL
Beaker Desiccant
Fittings
Locking Screws
On/Off Button
Balance Interface Connector
External
Magnetic Stirrer
KF Electrode
Input
PC Interface
SETUP
1.4.3. TITRATOR LEFT VIEW
2-6
Printer Connector
PC Keyboard
Connector
Power Adapter
Connector
1.4.4. TITRATOR ASSEMBLY
Note: Assembly operations must be completed before connecting the titrator to the power supply!
INSTRUCTION MANUAL
1.4.4.1. CONNECTING THE PUMP
To connect the dosing pump, follow these steps:
• Retrieve the pump cable from inside the left bay.
• Connect the cable to the pump as shown below (A). The pump connector is located on the bottom of the pump.
• Lower the pump into the titrator (B), then slide it towards the front of the titrator case until it is firmly latched.
• Secure the pump with the locking screw (C).
2
B
A
C
SETUP
1.4.4.2. CONNECTING THE AIR PUMP AND MAGNETIC STIRRER
To connect the air pump and magnetic stirrer, follow these steps:
• Retrieve the air pump cable from inside the right bay.
• Connect the cable to the air pump as shown below (A). The air pump and magnetic stirrer is located on the
bottom of the assembly.
• Lower the pump into the titrator (B), then slide it towards the front of the titrator case until it is firmly latched.
• Secure the pump with the locking screw (C).
B
C
A
2-7
1.4.4.3. ATTACHING THE BURETTE
Make sure that the mark from the valve actuating cap and the burette body are aligned as shown below.
INSTRUCTION MANUAL
2
SETUP
While ensuring the correct coupling between the syringe plunger (A) and the pump piston (B), slide the burette into the
support on the burette pump.
2-8
2
INSTRUCTION MANUAL
1.4.4.4. ASSEMBLING THE BEAKER
To attach the beaker assembly follow the steps below:
• Align the beaker support (D) with the base plate and attach by rotating clockwise.
• Place beaker ring (C) onto beaker support (D) with the notches on top.
• Insert the glass beaker (B) into the beaker ring (C).
• Add the stir bar to the glass beaker (B).
• Carefully place the beaker top (A) onto the beaker (B). Secure in place by pushing the beaker top through the
beaker ring (C) with the 4 notches of the beaker ring aligned with the 4 steel pins of the beaker top.
• Twist the beaker ring (C) counter-clockwise to lock the top in place.
A
B
C
SETUP
D
Hi933
SCALE 1:2
2-9
SETUP
INSTRUCTION MANUAL
2
1.4.4.5. BEAKER TOP
Warning! Do not overtighten fittings! This may cause permanent damage to o-rings and beaker top!
To assemble the beaker top follow the steps below:
1.4.4.5.1. ANTI-DIFFUSION DISPENSING TIP AND DISPENSING TUBE
To install the anti-diffusion tip and dispensing tube follow the steps below:
• Push dispensing tip (A) through the dispensing tip o-ring (B) until the o-ring is at the lip of the dispensing tip.
Insert the tip through the proper port (the HI933 ships with the dispensing tip and o-ring installed).
• Position the tip so that the angled portion is directed toward the center of the assembly.
• Fasten the dispensing tube (C) from the burette assembly to the dispensing tip port using the fitting. Ensure that
the tip remains oriented toward the center of the beaker.
1.4.4.5.2. KARL FISCHER ELECTRODE
To install the Karl Fischer electrode in the beaker top follow the steps below:
• Carefully insert the electrode (D) through a 10-mm fitting (E) and 10-mm o-ring (F).
• Insert electrode through proper port in beaker top.
• Align the pins to the center of the beaker, fasten the 10-mm fitting (E) to the beaker top. The electrode should
be as far down into the beaker as possible without touching the stir bar.
1.4.4.5.3. SOLVENT HANDLING SYSTEM
To attach solvent bottle tubing or waste bottle tubing, follow the steps below:
• Loosen the 5-mm fitting (H) on the solvent and/or waste port.
• Remove the desired plug or plugs (G).
• Insert the blue PTFE tubing from the solvent and/or waste bottle assemblies through the 5-mm fittings (H) and
o-rings (I) until about 1 cm of tubing is visible inside the beaker.
• Tighten the 5-mm fittings (H) until snug. This will cause the o-rings (I) to seal around the tubes.
2-10
1.4.4.5.5. DESICCANT CARTRIDGE
• Insert the stem of a desiccant cartridge (M) without hose-barbed cap (N) through a 10-mm fitting (E) and 10mm o-ring (F).
• Insert in the proper port of the beaker top.
• Fasten to the beaker top with the 10-mm fitting.
2
INSTRUCTION MANUAL
1.4.4.5.4. SAMPLE PORT PLUG
The HI933 is delivered with the sample port plug assembled and installed. To replace the rubber septum, follow the
steps below:
• Insert a red rubber septum (J) into the septum holder (K).
• Secure the septum with a 10-mm fitting (E).
• Place the sample port plug o-ring (L) on the bottom of the septum holder (K).
• Insert the assembled sample port plug into the dedicated port of the beaker top.
1.4.4.5.6. ELECTRICAL CONNECTIONS
• Connect the KF electrode to the BNC connector (A).
• Connect the power adapter cable to the power input connector (D).
SETUP
A
B
C
D
E
F
G
H
Function
Detector
Stirrer
USB interface
Power input connector (24VDC)
External PC keyboard
Printer
RS232 interface (Balance Interface)
Power switch
Type of Connector
BNC socket
6-pin Connector
USB Standard B
DC Power Jack connector
6-pin Mini Din (Standard PS2)
DB-25 Socket
DB-9 Socket
2-11
SETUP
INSTRUCTION MANUAL
2
1.4.4.6. TITRANT, SOLVENT, WASTE BOTTLE ASSEMBLY
The bottle top assemblies are equipped with desiccant cartridges containing indicating silica gel which ensures that the
air passing through the solvent handling system has been dried.
The desiccant has a limited capacity to absorb moisture and is typically exhausted after 2 to 4 weeks. Silica gel,
indicating or otherwise, can be regenerated at 150 °C.
The bottle tops are made of PTFE and have been designed to accommodate reagent bottles with GL-45 type threaded
tops.
The waste and solvent bottle top assemblies include blue PTFE tubing for the handling of liquid Karl Fischer solvent and
a clear flexible silicone based tubing for use with the air pump.
1.4.4.6.1. TITRANT BOTTLE ASSEMBLY (HI900530)
Caution: Most Karl Fischer titrants give off harmful vapors. Consult manufacturer’s
MSDS for safe handling guidelines.
To assemble the titrant bottle, follow the steps below:
• Insert PTFE top (J) into a GL45 screw cap (E).
• Insert a desiccant cartridge (B) without hose-barbed cap (A) through a 10-mm
fitting (F) and 10-mm o-ring (G).
• Insert and screw the desiccant cartridge assembly into the corresponding hole in
the white PTFE top (J). Fasten with 10-mm fitting (F).
• Ensure that the tube protector (C) is installed on the aspiration tubing (D).
• Insert the burette aspiration tubing (D) in the corresponding 3-mm fitting (H) and
attach the 3-mm o-ring (I).
• Insert and screw the aspiration tube fitting into the corresponding hole in the cap.
• Push the aspiration tubing fully into the titrant bottle until only the tube protector
(C) is visible outside of the titrant bottle (K).
• Screw GL45 cap (E) with full assembly onto the titrant bottle (K).
1.4.4.6.2. SOLVENT AND WASTE BOTTLE ASSEMBLY (HI900531)
Caution: Most Karl Fischer solvents give off harmful vapors. Consult manufacturer’s
MSDS for safe handling guidelines.
To assemble the solvent or waste bottle, follow the steps below:
• Insert a PTFE top (J) into a GL45 cap (E).
• Screw on the desiccant cap with screw hose barb (A).
• Insert a desiccant cartridge (B) with hose-barbed cap (A) through a 10-mm
fitting (F) and 10-mm o-ring (G).
• Insert and screw the desiccant fitting into the corresponding hole. Fasten the
desiccant cartridge assembly to PTFE top (J) with 10-mm fitting (F).
• Insert the solvent / waste tube (D) in the 5-mm fitting (H) and attach the o-ring (I).
• Insert and screw the tube fitting into the corresponding hole in the cap.
• Screw GL45 (E) cap with full assembly onto titrant bottle (K).
• Add the air tube (C) to the desiccant cap (A) and connect it to the corresponding
position on the air pump. The “Fill” position connects to the solvent bottle
assembly. The “Empty” position connects to the waste bottle assembly.
2-12
2
2. USER INTERFACE
2.1. START UP
INSTRUCTION MANUAL
Once the instrument is assembled and installed, follow the steps below to start the titrator:
• Connect the titrator to a power outlet with the supplied power adapter.
• Turn on the titrator from the power switch located on the back of the instrument.
• Wait until the titrator finishes the initialization process.
• Press
when prompted or wait a few seconds for titrator to start.
Note: All the performed initialization processes must be successfully completed. If one of the initialization processes
fails, restart the titrator. If the problem persists contact your nearest Hanna Instruments Service Center.
2.2. KEYPAD
USER INTERFACE
The titrator’s keypad is grouped into five categories, as follows:
Numeric
Keys
Function
Keys
Arrow
Keys
Option Keys
Enter Key
2-13
INSTRUCTION MANUAL
2
2.2.1. FUNCTION KEYS
If one of these keys is pressed, the associated function is immediately performed. Some of the keys are active only in
specific screens:
Starts or Stops a titration process
Turns the selected stirrer On and Off
Reserved
Access the Data Parameters Menu (reports, GLP, meter information, report setup)
Displays Contextual Help
2.2.2. OPTION KEYS
These keys are assigned to the virtual keys on the display. Their functions are listed in the boxes above the buttons and
vary depending on the displayed screen.
An underlined virtual key can also be activated by pressing
.
USER INTERFACE
2.2.3. ARROW KEYS
These keys have the following functions:
• Move the on-screen cursor.
• Increase and decrease the stirrer speed and other settings.
• Select a character (alphanumeric screen only).
• Navigate through menu options.
2-14
2.2.4. NUMERIC KEYS
Keys to
Used for numeric entries.
Toggles between positive and negative values.
Used for decimal point.
2.2.5. ENTER KEY
This key has the following functions:
• Accepts alphanumeric data entry.
• Executes the default (underlined) virtual option key.
2.3. DISPLAY
Process stage icon
Process status
Time and Date
Method name
Process stage
Burette icon
Last dose volume
Stirrer speed
Reminders or Messages
Pre-titration/Titration volume
mV value
INSTRUCTION MANUAL
The titrator has a large color graphical display. The main screen is shown below with short explanations of the screen
segments.
2
Drift value
Virtual option keys
The user interface contains several screens. For each titrator function, several screens may be used.
2.3.1. THE IDLE SCREEN
After start up and initialization, the first screen displayed is the Idle screen.
USER INTERFACE
Idle screen fields:
Method name:
Displays the name of the selected method.
Time and date:
Displays the current date and time.
Stirrer information: Actual / Set stirrer speed is displayed in RPM. When stirrer is off, the stirrer information is not
displayed.
Titrant:
Displays the name of the current titrant.
Last Standardization: Displays the titrant standardization date and time.
Reminders:Indicates when a task needs to be performed and displays error or warning messages.
2-15
USER INTERFACE
INSTRUCTION MANUAL
2
2.3.2. THE PROCESS SCREEN
When the user presses
screen.
while in Idle, all titration related processes are started. The titrator displays the Process
Process screen fields:
Method name:
Displays the name of the selected method.
Time and date:
Displays the current date and time.
Process stage field:Displays the current process (Pre-titration, Drift Analysis, Standby, Sample Analysis / Titrant
Standardization).
Process status:
Displays the process status with a descriptive drawing.
mV reading:
Displays the KF electrode potential.
Dispensed titrant:
Displays the total volume of dispensed titrant.
Last dose:
Displays the last titrant dose volume.
Drift value:
Displays the drift value (when available).
Stirrer information:
Actual / Set stirrer speed is displayed in RPM.
Burette status: A descriptive drawing is displayed indicating the burette is active and cannot be removed.
Reminders:
Indicates when a task needs to be performed and displays error or warning messages.
2.4. MENU NAVIGATION
2.4.1. SELECTING AN OPTION
To select an option, press the option key below the virtual key. For example,
to access the Method Options screen press the option key below it.
2-16
2.4.2. SELECTING A MENU ITEM
2.4.3. ENTERING TEXT
INSTRUCTION MANUAL
To select an item from the menu screen, use the arrow keys and to
move the cursor.
When the menu is larger than the display, a scroll bar is active on the right
side.
To activate the selected menu item, press
or
.
2
To enter text in an alphanumeric input box, first erase the previous text by
using
.
To enter a letter, highlight it using the arrow keys then press
. Use the
same procedure to enter the whole name.
For editing, use the
and
keys.
When editing is complete, press
.
The method name will be updated and displayed in the name field of the
View/Modify Method screen.
When all the desired parameters have been set, press
.
USER INTERFACE
2.4.4. SAVING MODIFICATIONS
The Saving Method screen allows the user to save the modifications. To
exit without saving, press
or highlight Exit Without Saving Method
option and then press
. To save the modifications highlight Save
Method option and then press
.
Note: To access the contextual help menu, press
at any time. Help is related to the displayed screen. Press
or
to return to the previous screen.
2-17
INSTRUCTION MANUAL
2
3. GENERAL OPTIONS
The General Options screen gives access to options that are not directly related to the titration process. In Idle mode,
on the main screen press
to access this screen. In Pre-titration, Standby or during a Titration, press the
<<Home>> key on a PS/2 keyboard to access this screen.
3.1. SAVE FILES TO USB STORAGE DEVICE
Note: The USB Storage Device has to be formatted FAT or FAT32.
GENERAL OPTIONS
This option allows the user to save files from the titrator to a USB storage device.
On the titrator, the available file types are:
Standard Method Files
HIXXXXYY.MTD (e.g.: HI8001EN.MTD, HI8101EN.MTD)
User Method Files
USERXXXX.MTD (e.g.: USER0001.MTD)
Drift/Titration Report Files
-DR_xxxxx.RPT, KF_xxxxx.RPT (e.g.: DR_00001.RPT, KF_00001.RPT)
Insert the USB storage device into the USB port on the right side of the titrator.
Use the and keys to select the file type. The number of files and the file names will be displayed.
Use the and keys to scroll through the list.
2-18
Note: The saved files will be stored on the USB key in the HI933 folder, as follows:
• Methods: USB Drive\HI933\Methods\*.mtd
• Reports: USB Drive\HI933\Reports\*.rpt
3.2. RESTORE FILES FROM USB STORAGE DEVICE
This screen allows the user to transfer files from the USB storage device to the titrator.
GENERAL OPTIONS
The file types that can be transferred are:
Standard Method Files
HIXXXXYY.MTD (e.g.: HI8001EN.MTD, HI8101EN.MTD)
User Method Files
USERXXXX.MTD (e.g.: USER0001.MTD)
Drift/Titration Report Files
-DR_xxxxx.RPT, KF_xxxxx.RPT (e.g.: DR_00001.RPT, KF_00001.RPT)
Insert the USB storage device into the USB port on the right side of the titrator.
Use the and keys to select the file type. The number of files and the file names will be displayed.
Use the and keys to scroll through the list.
The option keys allow the following operations:
Returns to the General Options screen.
Copies the highlighted file from the USB storage to the titrator.
Copies all currently displayed files from the USB storage to the titrator.
Deletes the highlighted file.
Deletes all currently displayed files.
2
INSTRUCTION MANUAL
The option keys allow the following operations:
Returns to the General Options screen.
Copies the highlighted file from the titrator to the USB storage device.
Copies all currently displayed files from the titrator to the USB storage device.
Deletes the highlighted file.
Deletes all currently displayed files.
Note: In order to restore files from USB Key, please ensure that the methods and/or reports you wish to transfer to
the titrator are in the correct folder:
• Methods: USB Drive\HI933\Methods\*.mtd
• Reports: USB Drive\HI933\Reports\*.rpt
2-19
INSTRUCTION MANUAL
2
3.3. STANDBY MODE
Option: Disabled or Enabled
When enabling this option the titrator will return to Standby mode automatically after the titration has been completed.
3.4. STANDBY DURATION
GENERAL OPTIONS
Option: 10 minutes to 72 hours
The user can enter the period of time for which the cell is kept dry and ready for subsequent analysis after a titration
has finished.
The external stirrer is automatically detected when it is connected.
2-20
3.5. TITRANT DATABASE
This screen allows the user to store information about titrants, including the name and standardization information.
2
INSTRUCTION MANUAL
The titrant for the currently-selected method cannot be modified from this screen. For details on the full functionality of
the database,see Method Options section.
3.6. STANDARD DATABASE
This screen allows the user to store information about standards, including the name and concentration.
GENERAL OPTIONS
The standard for the currently selected method cannot be modified from this screen. For details on the full functionality
of the database, see Method Options section.
2-21
INSTRUCTION MANUAL
2
3.7. ESTIMATED CELL VOLUME
Option: 0.0 mL to 200.0 mL
Use the numeric keypad to enter the estimated volume of solution in the titration beaker.
3.8. USB LINK WITH PC
GENERAL OPTIONS
In order to use this feature, the USB cable needs to be connected from the titrator to the PC. Make sure that HI900 PC
application is running on the PC.
“Active/Inactive” shows the status of the USB link with the PC.
“Active” means that the titrator is using the USB communication with the PC and not with another device.
“Ready” shows that the titrator is able to communicate with the PC.
During transfer of any information between the PC and the titrator, “Transmit” and the status is displayed.
Note: To allow our users access to the latest version of Hanna Instruments PC compatible software, we made
the products available for download at http://software.hannainst.com. Select the product code and click
Download Now. After download is complete, use the setup.exe file to install the software.
2-22
3.9. SETUP BALANCE INTERFACE
INSTRUCTION MANUAL
This screen allows the user to setup an analytical balance for automatic acquisition of sample mass prior to titration or
standardization.
2
The balance is connected to the titrator via RS 232 interface.
Enables the selected balance.
Disables the selected balance (automatic weight acquisition will be not available).
Returns to the General Options screen.
Adds a new balance to the list.
Customizes the serial communication parameters. The Balance Configuration screen will open.
Deletes the highlighted balance.
Be sure that the balance configuration settings match the settings for your balance (baud rate, data bits, parity, stop bit
number, request command syntax). It may be necessary to change settings on your balance. Users should consult their
balance instruction manual.
Before leaving this screen be sure the connection with the balance is working properly by pressing the
key.
GENERAL OPTIONS
Note: At least one balance must be in the list.
2-23
INSTRUCTION MANUAL
2
3.10. STIRRER
Option: Internal, External, Custom
This screen allows the user to select the internal magnetic stirrer, an external magnetic stirrer or a user-controlled stirrer
(custom).
3.11. PRINTER MODE
GENERAL OPTIONS
Option: Ansi, Ascii, Text
Ansi mode: U se this mode when the printer is set as Ansi. In this case all the accented characters/symbols available in
titrator will be printed on the printer.
Ascii mode: U se this mode when the printer is set as Ascii. In this case only some of the accented characters/symbols
available in titrator will be printed on the printer.
Text mode: This mode is recommended when the user doesn’t need to print accented characters.
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3.12. DATE AND TIME SETTING
INSTRUCTION MANUAL
This screen allows the user to set the date and time.
Use the and keys or the numeric keys to modify the date and time.
Press
to move the cursor to the next field.
Press
or
to change the time format.
2
3.13. DISPLAY SETTINGS
GENERAL OPTIONS
This screen allows the user to customize the display settings.
Option Keys:
Increases the backlight saver time interval
Decreases the backlight saver time interval
The backlight intensity can be adjusted using the and keys.
There are 8 levels of backlight intensity, ranging from 0 to 7.
The displayed color palette allows for selection of appropriate backlight intensity.
The backlight saver option protects the display during standby periods, when no keys have been pressed for a set amount
of time.
If the backlight is off, any keystroke will re-activate the backlight without performing any action.
The range for backlight saver interval is between 1 and 60 minutes. To disable the backlight saver increase the time to
the maximum allowed. The “Off” indication will appear.
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INSTRUCTION MANUAL
2
3.14. BEEPER
Option: On or Off
If enabled (on) an audible alert will sound after a titration is completed, when an invalid key is pressed or when a critical
error occurs during titration.
3.15. LANGUAGE
GENERAL OPTIONS
Option: English, Español, Português, Français
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3.16. CALIBRATION CHECK
This screen allows the user to verify the electrode mV input and the electrode polarization current.
2
INSTRUCTION MANUAL
3.17. RESET TO DEFAULT SETTINGS
GENERAL OPTIONS
The electrode mV input and the electrode polarization current are measured with the HI900941 calibration key and a
mV/µA multimeter (not included).
Disconnect the KF electrode, then connect the HI900941 calibration key to the electrode input (BNC connector).
To check the mV input:
Set the multimeter to mV mode.
Switch the calibration key to mV mode by pressing the red button.
Connect the calibration key banana plugs to the multimeter mV input.
Use the and keys to change the imposed current (predefined list).
The millivolt reading displayed on the titrator screen should be within 2% of the reading on the multimeter.
To check the μA output:
Set the multimeter to μA mode.
Switch the calibration key to μA mode by pressing the red button.
Connect the calibration key banana plugs to the multimeter mA input.
The reading on the multimeter should be in accordance with the prescribed µA value on the titrator screen.
Note: This will delete all the user methods and restore all manufacturer settings such as titrator configuration,
standard method parameters, etc.
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INSTRUCTION MANUAL
2
3.18. OPTIMIZE MEMORY SPACE
This screen allows the user to run a memory defragmentation utility in order to increase the speed to the strage memory
access. Press
and then restart the titrator. Do not disconnect the power suply during this operation.
3.19. UPDATE SOFTWARE
GENERAL OPTIONS
This screen allows the user to update the titrator software from a USB storage device containing a software setup kit.
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To update the software:
• Copy the “Setup933” folder to a USB storage device.
• Insert the USB storage device into the titrator.
• Go to General Options, then Update Software. The titrator will display the current and new software versions.
• Press
. When prompted, remove the USB storage device and restart the titrator.
2
4. TITRATION METHODS
4.1. SELECTING METHODS
To select a method, press
from the main screen. A list of available methods will be displayed.
TITRATION METHODS
In the Titration Methods screen, you can view the list of all available methods (standard and user methods).
To select a method, highlight the method then press
, the name of the selected method will be displayed on
the main screen.
INSTRUCTION MANUAL
All parameters required to complete an analysis are grouped into a method.
The titrator is supplied with a pack of standard methods, these methods have been developed by Hanna Instruments
and can be used to create user methods.
Standard and user methods can be upgraded, saved or deleted by connecting the titrator to a PC using the HI900 PC
application or a USB flash drive.
4.2. STANDARD METHODS
The standard methods are developed for the most common types of analysis.
Only specific method parameters can be modified by the user (see Method Options section).
Also, standard methods can be used as a template to create new user methods.
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TITRATION METHODS
INSTRUCTION MANUAL
2
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4.2.1. UPGRADING STANDARD METHODS
To upgrade the titrator with new standard methods, follow the steps below:
From USB storage device:
• Insert the USB storage device into the USB port, located on the right side of the titrator.
• Press
from the main screen.
• Using and keys, highlight Restore from USB Storage Device option and choose
.
• Using
and
keys, navigate through file types to find “standard method files”. The list with available
standard methods will be displayed.
• Press the
or
key to upgrade the titrator with the standard methods.
• Press
to return to General Options screen.
From PC:
You can upgrade the titrator with standard methods from a PC using the HI900 PC application (see General Options
section).
4.2.2. DELETING STANDARD METHODS
Unnecessary standard methods can be removed from the titrator by following the procedure below:
From General Options Screen:
• Using the and keys, highlight Save to USB option and press
.
• Using the and keys, navigate through the file types menu to find “standard method files”. The available
standard methods will be displayed.
• Press the
or
keys to remove unnecessary standard methods.
• Press
to return to the General Options screen.
From PC:
Unnecessary standard methods can be removed from the titrator using the HI900 PC application (see General Options
section).
4.2.3. RESTORING THE STANDARD METHODS TO THE MANUFACTURER SETTINGS
You can restore the standard methods to the default settings by highlighting a standard method and pressing
.
4.3. USER METHODS
4.3.1. CREATING USER METHODS
To create a new user method, start from a standard or previously generated user method and follow these steps:
• Press
from the main screen.
• Using the and keys, highlight an existing method from the method list.
• Press
. A new user method will be generated.
• Press
to activate the recently generated user method.
4.3.2. DELETING USER METHODS
To remove a user method, press
from the main screen. Highlight the user method that you want to delete and
press
. A screen will appear in order to confirm the deletion. Press
again to confirm, or press
to cancel the operation.
TITRATION METHODS
Note: Only a limited number of methods can be installed on the titrator. The titrator can hold 100 methods (standard
and user). When the limit is reached, a warning message is displayed.
INSTRUCTION MANUAL
These methods are defined by the user (usually by modifying a standard method).
The user methods can be developed in accordance with the requirements of the user. All method parameters can be
modified by the user.
2
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INSTRUCTION MANUAL
2
4.4. VIEWING / MODIFYING METHOD
To modify the method parameters, press
method will be displayed. Press the and
from the main screen. A list of all the parameters for the selected
keys to highlight the option you want to modify and choose
.
TITRATION METHODS
To exit the View/Modify Method screen, press the
modifications.
Press
to discard the changes.
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key, and highlight Save Method and press
to save
4.5. METHOD OPTIONS
2
Note: Only certain method options can be changed for standard methods.
INSTRUCTION MANUAL
4.5.1. NAME
Option: Up to 24 characters
4.5.2. METHOD REVISION
Option: Up to 3 characters
TITRATION METHODS
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4.5.3. METHOD TYPE
Option: Sample Analysis or Titrant Standardization
INSTRUCTION MANUAL
2
TITRATION METHODS
4.5.4. PREDISPENSING AMOUNT
Option: 0% to 90%
If the approximate water content is known, the titration time can be shortened by adding a large fraction of the titrant
at the start.
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To disable this feature set the predispensing amount to 0%.
2
INSTRUCTION MANUAL
4.5.5. PRE-ANALYSIS STIR TIME
Option: 0 to 1000 seconds
To avoid erroneous results or unreachable end points when analyzing samples with limited solubility, the sample must
be completely dissolved in the solvent prior to the start of a titration.
After the sample has been added to the titration beaker, the titrator will stir for the set period of time before any titrant
(excluding predispensing) is added to the cell.
4.5.6. STIRRER SPEED
Option: 200 to 2000 RPM
TITRATION METHODS
The stirrer will remain on for as long as the method is active. When the stirrer is running, the speed can be adjusted at
any time by using the and keys.
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4.5.7. STIRBAR TYPE
Option: Up to 10 characters
INSTRUCTION MANUAL
2
TITRATION METHODS
4.5.8. DRIFT ENTRY
Option: Automatic or User
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Automatic: The drift rate will be calculated automatically after the pre-titration of the solvent.
User:The drift is set to a fixed value (entered by the user). The user enters the estimated drift value. The drift
analysis stage will be skipped.
4.5.9. SOLVENT NAME
Option: Up to 15 characters
2
INSTRUCTION MANUAL
4.5.10. SAMPLE PARAMETERS (SAMPLE ANALYSIS ONLY)
This screen allows the user to configure parameters for the sample to be analyzed.
TITRATION METHODS
4.5.10.1. SAMPLE DETERMINATION
Option: Normal, External Extraction, External Dissolution
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INSTRUCTION MANUAL
2
Normal: The analysis is performed through direct titration of the sample. The sample is soluble in the solvent or finely
divided with a homogeneous distribution of water.
External extraction:
The sample is insoluble in the solvent and an external water extraction is necessary.
External dissolution: The sample has very high water content, non-homogeneous water distribution, or is slow to
dissolve. The sample is dissolved in a separate container and then a small amount of the
solvent is titrated.
See Optimization section for further details.
4.5.10.1.1. NORMAL
TITRATION METHODS
Sample Name
Option: Up to 15 characters
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Sample Type
Option: Mass, Volume, Pieces
2
INSTRUCTION MANUAL
Sample Size
Option: 0.0010 to 100.0000 g, 0.0010 to 100.0000 mL, 1 to 100 pcs.
TITRATION METHODS
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Sample Density (by volume only)
Option: 0.200 to 3.000 g/mL
INSTRUCTION MANUAL
2
TITRATION METHODS
4.5.10.1.2. EXTERNAL EXTRACTION
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Sample Name
Option: Up to 15 characters
Sample Size
Option: 0.0010 to 100.0000 g
2
INSTRUCTION MANUAL
External Solvent Size
Option: 0.0010 to 100.0000 g
TITRATION METHODS
External Solvent Concentration
Option: 0.0100 to 100.0000 %
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Extracted Sample Size
Option: 0.0010 to 100.0000 g
INSTRUCTION MANUAL
2
TITRATION METHODS
4.5.10.1.3. EXTERNAL DISSOLUTION
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Sample Name
Option: Up to 15 characters
Sample Size
Option: 0.0010 to 100.0000 g
2
INSTRUCTION MANUAL
External Solvent Size
Option: 0.0010 to 100.0000 g
TITRATION METHODS
External Solvent Concentration
Option: 0.0100 to 100.0000 %
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Dissoluted Sample Size
Option: 0.0010 to 100.0000 g
INSTRUCTION MANUAL
2
TITRATION METHODS
4.5.11. STANDARD (TITRANT STANDARDIZATION ONLY)
This screen allows the user create a database with standards and customize related parameters.
Using the and keys, highlight the standard from the existing list and press
to choose it.
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Press
Press
Press
Press
Press
it you want to use the selected standard for the titrant standardization.
to return to the View/Modify Methods screen.
if you want to edit the Karl Fischer standard parameters.
if you want to create and add a new standard to the Karl Fischer standard data base.
if you want to remove a Karl Fischer standard from the pre-defined list.
2
INSTRUCTION MANUAL
Titrant standardization methods supplied by Hanna are designed to be used with specific standards. The HI933 will
automatically select an appropriate standard when such a method is selected. If this standard is not in the database, a
new one will be created.
4.5.11.1. STANDARD NAME
Option: up to 15 characters
TITRATION METHODS
4.5.11.2. STANDARD TYPE
Option: Solid by mass, Liquid by mass, or Liquid by volume
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4.5.11.3. CONCENTRATION UNIT
Option: %[W/W], ppm, mg/g or mg/mL
INSTRUCTION MANUAL
2
TITRATION METHODS
4.5.11.4. WATER CONTENT
Option: 0.0100 to 1000.0000 mg/g
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2
INSTRUCTION MANUAL
4.5.11.5. STANDARD SIZE
Option: 0.0010 to 50.0000 g
Use the numeric keypad to enter the size (g or mL) to be used in the standardization.
When a new standardization is started the titrator will prompt for the exact mass or volume. The standard size can be
acquired automatically from a compatible balance when this feature is enabled.
4.5.11.6. STANDARD DENSITY (LIQUID BY VOLUME ONLY)
Option: 0.200 to 3.000 g/mL
TITRATION METHODS
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INSTRUCTION MANUAL
2
4.5.12. TITRANT
The user can access the Karl Fischer titrant database and customize related parameters.
Using the and keys, highlight the titrant from the existing list and press
it you want to use the selected titrant for the titrant standardization.
to return to the View/Modify Methods screen.
to edit the titrant parameters.
to create a new titrant.
to remove the titrant from the database.
TITRATION METHODS
Press
Press
Press
Press
Press
to choose it.
Titrant standardization methods supplied by Hanna are designed to work with specific titrant concentrations. The HI933
will automatically select an appropriate titrant when such a method is selected. If there is no usable titrant in the
database, a new one will be created.
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4.5.12.1. TITRANT NAME
Option: up to 15 characters
2
INSTRUCTION MANUAL
4.5.12.2. TITRANT TYPE
Options: One-component, One-component (Ketone/Aldehyde), Two-components (Methanol), Two-components
(Ethanol) or Others
TITRATION METHODS
4.5.12.3. NOMINAL TITRANT CONCENTRATION
Option: 0.0010 to 20.0000 mg/mL
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4.5.12.4. STANDARDIZED TITRANT CONCENTRATION
INSTRUCTION MANUAL
2
TITRATION METHODS
4.5.12.5. TITRANT AGE REMINDER
Option: Off, 0 to 31 days
A programmable reminder will appear when it is time to verify the titrant concentration or to change the titrant.
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4.5.13. CONTROL PARAMETERS
The user can access and edit the parameters related to the titration.
4.5.13.1. START MODE
Option: Cautious or Normal
2
INSTRUCTION MANUAL
Cautious: The titrant dosing begins with the minimum dose in order to prevent over-titration.
Normal:The titrant dosing begins with the median value between the minimum and maximum (i.e. minimum dose
5 μL, maximum dose 25 μL, first dose will be 15 μL).
4.5.13.2. IMPOSED CURRENT
Option: 1 µA, 2 µA, 5 µA, 10 µA, 15 µA, 20 µA, 30 µA, or 40 µA
Use the and keys to select the electrode polarization current from the predefined list.
TITRATION METHODS
Note: Higher polarization currents will speed the contamination of the electrode and potentially degrade samples.
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4.5.13.3. DOSING PARAMETERS
Option: 0.125 to 4000 µL
INSTRUCTION MANUAL
2
TITRATION METHODS
4.5.13.4. MAXIMUM DOSING MODE
Option: Disabled or Enabled
When enabled, the titrator will use a dosing algorithm which ensures a faster titration by changing the dosing mode if
the mV is far from the end point.
The algorithm will use maximum dosing if the difference between mV value and end point is higher than 150 mV.
Disable this option if higher accuracy is desired.
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4.5.13.5. TIMED INCREMENT
Use the and keys to enter the period of time between two successive doses.
2
INSTRUCTION MANUAL
4.5.13.6. END POINT VALUE
Option: 5.0 to 600.0 mV
Use the numeric keypad to enter the mV value at which the titration equivalence point (end point) has been reached.
This value is also used to determine when the pre-titration is complete.
TITRATION METHODS
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INSTRUCTION MANUAL
2
4.5.13.7. SIGNAL AVERAGING
Option: 1 to 10 readings
The titrator will take the last reading and place it into a “moving window” along with the last 2, 3, etc readings
(depending on selected option). The average of these readings is displayed and used for calculations. Averaging more
readings is helpful when a noisy signal is received from the electrode.
If 1 reading is selected this option is disabled.
TITRATION METHODS
4.5.13.8. FLOW RATE
Option: 0.3 to 10.0 mL/min (for 5 mL burette)
Note: The titrator will automatically detect the burette size and display the correct high limit volume.
The flow rate is set for all burette operations.
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4.5.14. TERMINATION PARAMETERS
This screen allows the user to set the control parameters related to titration termination.
2
INSTRUCTION MANUAL
4.5.14.1. MAXIMUM DURATION
Option: 10 to 3600 seconds
If the titration end point is not reached, the titration will be terminated after the maximum duration. The error message
“Value Out of Range” will appear on the display.
TITRATION METHODS
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INSTRUCTION MANUAL
2
4.5.14.2. MAXIMUM TITRANT VOLUME
Option: 0.100 to 50.000 mL
The maximum titrant volume used in the titration must be set according to the analysis. If the titration end point is
not reached, the titration will be terminated after the maximum titrant volume has been dispensed. The error message
(“Limits Exceeded”) will appear on the display.
TITRATION METHODS
4.5.14.3. TERMINATION CRITERION
Option: mV End Point, Absolute Drift or Relative Drift
mV End Point The titration is terminated when the potential remains below a set end point value for a specified
period of time.
Absolute Drift The titration is terminated when the actual drift is less than the predefined absolute drift value.
Relative Drift The titration is terminated when the actual drift is less than the sum between the initial drift and the
predefined relative drift.
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2
INSTRUCTION MANUAL
4.5.14.4. END POINT STABILITY TIME
Option: 1 to 30 seconds
The potential must remain below the set end point value for the specified period of time.
4.5.14.5. ABSOLUTE DRIFT
Option: 0.0 to 40.0 µg/min
TITRATION METHODS
4.5.14.6. RELATIVE DRIFT
Option: 0.0 to 40.0 µg/min
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4.5.15. RESULT UNIT
Option: %, ppm, mg/g, µg/g, mg, µg, mg/mL or µg/mL
INSTRUCTION MANUAL
2
TITRATION METHODS
4.5.16. SIGNIFICANT FIGURES
Option: Two (XX), Three (XXX), Four (XXXX) or Five (XXXXX)
This option allows you to set the format for displaying the final titration result.
4.6. PRINTING
To print method parameters, press
from the main screen.
Press
and wait a few seconds until the printer completes the job.
If no printer is connected to the dedicated socket, or if the printer is offline, an error message will appear on the display
(see Connecting a Printer section, for details on connecting a printer to the titrator).
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5. TITRATION MODE
2
5.1. IDLE
TITRATION MODE
The titration (Sample Analysis or Titrant Standardization) is performed with the selected method.
Be sure that the selected method is customized in accordance with the specifics of the application.
Before performing a titration make sure that the following conditions are met:
• All of the attached systems (e.g.: solvent system) are properly assembled.
• The right amount of solvent is present in the beaker (between the min and max marks) for best reproducibility.
The following intermediary stages are performed automatically before starting the titration:
• Solvent pre-titration
• Drift analysis (Automatic Determination Entry only)
When the drift analysis process is finished, the titrator enters Standby mode. At this point, a titration can be initiated.
INSTRUCTION MANUAL
The titrator first enters Idle mode when it is switched on. All of the HI933’s software features and settings can be
accessed from the Idle mode. This includes all of the user-adjustable method parameters, solvent handling system, file
transfers, calibration checks, software upgrades, options for interface with PC and accessories as well as burette options.
To access the titration menu (Process screen) press
.
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INSTRUCTION MANUAL
2
5.2. PRE-TITRATION
In pre-titration, the residual water on the interior surface of the titration vessel, the water contained in the entrapped air
and the small amount of water from the solvent is eliminated.
The HI933 reacts residual water by adding titrant until the specified endpoint potential is reached. This setting is
associated with the selected method. After the electrode potential has stabilized, the titrator moves into the Drift Rate
Determination Stage.
When the pre-titration is started, the stirrer is automatically turned on and the user cannot change the selected method
or access the method parameters.
TITRATION MODE
Note: If the pre-titration lasts longer than 30 minutes the titrator switches to Idle mode. Errors may have occurred in
your titration system (beaker is not properly sealed, wrong or missing titrant, unconnected or bad electrode,
etc.). Check the system and start the pre-titration again.
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5.3. DRIFT ANALYSIS (AUTOMATIC DETERMINATION ENTRY ONLY)
While in this mode the HI933 conducts a one minute analysis which determines the amount of moisture leaking into the
cell from the atmosphere. Despite the titration vessel being tightly sealed, water will still seep into the cell. The amount
of water that migrates into the cell per unit time is known as the background drift rate, or the drift rate.
The drift rate is determined by keeping track of the number of very small, successive doses of titrant required to maintain
the ‘dryness’ of the solvent over the course of a minute. The rate at which water leaks into the cell is then calculated and
reported by the HI933 in units of μg/min.
2
INSTRUCTION MANUAL
The HI933 will automatically subtract the drift rate from the titration results. This is important for titration accuracy when
analyzing samples with very low water content, where the amount of water that has leaked into the cell is a considerable
fraction of the total water titrated during the analysis.
When the drift becomes stable the titrator switches to Standby mode.
During the drift analysis, if the titrator cannot maintain cell dryness, the titrator reverts to pre-titration.
Note: If the drift entry mode is set as Manual Entry the drift analysis stage is skipped.
5.4. STANDBY
TITRATION MODE
After the drift rate has been determined, the HI933 moves into Standby mode. In standby mode the dryness of the
titration cell is maintained and the drift rate is continuously monitored and updated.
From Standby mode a sample analysis, titrant standardization or drift rate logging session can be started as well
as method selection, customization of method parameters, and general options (external keyboard only, by pressing
<<Home>>).
After an initial titrator setup and prior to the first titration or standardization, the drift rate should be allowed to settle
in Standby mode for 45 min. This ensures that the drift rate is stable and reflects the actual rate at which water vapor
is entering the cell rather than representing a slow drying of the air between the solvent and the top of the cell. The
stabilization can be verified by examining the drift rate vs. time curve which can only be accessed from standby mode.
During standby, if the drift becomes unstable, the titrator will switch back to Drift Analysis mode.
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INSTRUCTION MANUAL
2
5.5. SAMPLE ANALYSIS
While in Standby mode, press
.
Note: If the drift value is zero, a warning message appears to inform the user that the solvent may be overtitrated.
or to return to Standby mode by pressing
in
TITRATION MODE
The user can choose to continue the titration by pressing
order to wait until the drift is stabilized at a higher value.
If necessary, update the estimated concentration. This value is used to determine the pre-titration volume. The optimal
limits will be updated based on this value.
Follow the steps below to add the sample to the titration vessel and determine the sample size.
5.5.1. SAMPLE SIZE
5.5.1.1. MANUAL ENTRY
5.5.1.1.1. SAMPLE SIZE BY MASS
1) Measure the mass of the sample in a weigh boat or syringe.
2) Remove the sample plug from the top of the beaker to open the sample port, or insert the syringe needle through
the septum.
3) Rapidly add the sample through the sample port or through the septum. Pay attention not to get any sample on
the electrode or beaker wall.
4) Replace the sample plug or remove the syringe from the septum.
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5.5.1.1.2. SAMPLE SIZE BY VOLUME
1) Attach a long needle (approximately 6 cm for best control) to a precision-volume syringe large enough to hold at
least one complete sample volume.
2) Rinse the syringe and needle with sample several times by drawing in a small portion of sample, fully extending the
plunger, shaking to coat the syringe interior and expelling the sample into a waste collection container.
3) Draw enough sample into the syringe for at least one titration.
4) Dry the outside of the needle with a lint free wipe or tissue.
5) Insert the needle through the septum in the sample port. Push the syringe through the septum until the end of the
needle is approximately 1 cm from the surface of the solvent.
6) Steadily dispense the appropriate volume of sample ensuring that the sample is introduced directly into the solvent
and does not splash or spatter onto the wall of the titration vessel, electrode, or dispensing tip.
7) Draw a small amount of air from inside the cell into the syringe to ensure that no sample drops remain on the tip
of the needle.
8) Remove the syringe and needle from the septum taking care to not touch the needle to the solvent or other internal
cell components.
9) Enter the volume of the sample.
5.5.1.2. AUTOMATIC MASS ACQUISITION FROM ANALYTICAL (SAMPLE SIZE BY MASS ONLY)
The sample size can be automatically acquired from the balance when connected to the titrator using the RS232
interface.
TITRATION MODE
5.5.1.1.3. SAMPLE SIZE BY PIECES
1) Remove the sample plug from the beaker top to open the sample port.
2) Use a gloved hand, tweezers, or a weigh boat to add the appropriate number of pieces to the titration vessel.
3) Replace the sample plug.
4) Enter the number of pieces that were added to the titration vessel.
2
INSTRUCTION MANUAL
5) Determine the mass of the ‘empty’ weigh boat or syringe.
6) Calculate the mass of the sample added (subtract the mass of the emptied weigh boat or syringe from the mass of
the full weigh boat or syringe).
7) Enter the calculated mass of the sample.
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INSTRUCTION MANUAL
2
5.5.2. PROCEDURE
1) Place the syringe or the weigh boat containing the sample on the balance.
2) Wait until the reading has stabilized and press
.
3) Add the sample in the titrator vessel.
4) Place the empty syringe or weigh boat on the balance.
TITRATION MODE
5) Wait for the reading to stabilize and press
.
The titrator returns to the previous screen and the sample size is automatically updated.
Press
to begin the analysis.
Note: The user must make sure that the balance and the titrator are properly configured and the balance feature is
enabled (see Setup Balance Interface).
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2
5.5.3. SAMPLE ANALYSIS
INSTRUCTION MANUAL
Press
Press
to stop the titration manually and return to the Idle mode.
to stop the titration and return to Standby mode.
5.5.4. SUSPEND TITRATION
While the titration is in progress, you can temporarily stop it by pressing
titrant.
To continue the titration, press
.
. The burette will stop dispensing
5.5.5. VIEWING THE TITRATION CURVE
During a titration, the titration curve can be displayed on the Titration Graph screen, by pressing
ID report is also displayed inside the graph window.
. The titration
TITRATION MODE
5.5.6. RESULTS
When the end point is reached the titration is finished and the following screen is displayed.
This screen displays information about the titration (duration, drift value used for compensation, sample size, titrant
concentration, dispensed titrant volume, titration report ID).
Press
to see the titration report.
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INSTRUCTION MANUAL
2
Press
Press
to see the titration graph.
to print the report.
TITRATION MODE
5.5.7. SAMPLE ANALYSIS HISTORY
By pressing
, results will be added to the Sample Analysis History in order to obtain an average of titration
results.
Use the and keys to scroll the results list.
Use
to choose the samples that will be used for averaging.
Note: When there are no results selected, dashes will appear in the Average Sample Concentration and the Standard
Deviation fields.
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5.6. TITRANT STANDARDIZATION
While in Standby mode, press
.
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INSTRUCTION MANUAL
Note: If the drift value is zero, a warning message appears to inform the user that the solvent may be overtitrated.
5.6.1. ADDING THE STANDARD
The user must add the standard into the beaker and enter the standard size. The units of sample size are determined
by the method setting.
TITRATION MODE
Follow the same procedure as for adding samples (see Sample Analysis).
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5.6.2. START STANDARDIZATION
Press
to begin standardization.
INSTRUCTION MANUAL
2
Note: During titrant standardization the user has the same options as a sample analysis (see Sample Analysis).
TITRATION MODE
When the titrant standardization is finished the user has two options to update the titrant concentration:
By pressing
the titrant is updated with the current result.
By pressing
the user can average the titrant concentration using more results.
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Use the
Use
Press
2
INSTRUCTION MANUAL
5.6.3. AVERAGING TITRANT STANDARDIZATION RESULTS
By pressing
results can be added to the sample analysis history in order to obtain an average of titrant
concentration.
and keys to scroll the concentration results list.
to choose the titrant concentration results that will be used for averaging.
to update the concentration with the current average.
Note: When there are no results selected, dashes will appear in the average titrant concentration and the standard
deviation fields.
is not available.
TITRATION MODE
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2
6. AUXILIARY FUNCTIONS
AUXILIARY FUNCTIONS
INSTRUCTION MANUAL
6.1. AIR PUMP
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The air pump is used to add or remove the solvent in the titration beaker without exposure to atmospheric moisture.
To enter Air Pump screen, press
from the Idle screen.
6.1.1. FILLING THE BEAKER
To add solvent to the titration beaker:
1) Press
from the Air Pump screen, the air pump will start and solvent will be added to the beaker. If the
solvent is not flowing or is flowing very slowly, verify that the bottle top assemblies are properly assembled and
tightly sealed and that the liquid handling tubing reaches the bottom of the solvent bottle.
2) When the level of solvent inside the titration cell reaches the “Min” indicator line, press
to turn off the air
pump. If
is not pressed, the air pump will automatically shut off after 20 seconds.
3) The HI933 will prompt the user to verify that the titration cell has been filled to the “Min” line (approx. 50 mL)
Press
to return to the Idle screen.
6.2. BURETTE
To access the Burette screen, press
from the Idle screen.
Highlight the desired option and then press
.
6.2.1. PRIMING THE BURETTE
After solvent has been added to the titration cell, the burette can be primed with titrant. The priming process consists of
several cycles of filling and emptying the burette with titrant. It ensures that any air, water or water vapor in the burette
or tubing is removed.
Two rinse cycles of burette are shown in the figure below. The dispensing tube is connected on the right side and the
aspiration tube on the left side.
AUXILIARY FUNCTIONS
Note: Do not perform burette functions with solvent below the “Min” sign. Doing so could spray titrant on the beaker
top or other components.
2
INSTRUCTION MANUAL
6.1.2. EMPTYING THE BEAKER
To remove the waste from the titration beaker:
1) Loosen the waste tube fitting slightly and slide the waste tube down until it reaches the bottom of the beaker.
2) From the Air Pump screen, press
and allow the air pump to run until all of the waste has been removed.
3) Press
to turn off the air pump. If
is not pressed, the air pump will automatically shut off after 60
seconds.
4) Return the waste tube back into its original position and re-tighten the fitting.
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INSTRUCTION MANUAL
2
Note: Before starting this operation, the aspiration tube must be inserted into the titrant bottle.
To prime the burette, select Prime Burette from the Burette screen. Enter the number of rinses and press
.
The number of burette rinses can be set between 1 and 5 (we recommend at least three rinses to assure that the air
bubbles are completely removed).
AUXILIARY FUNCTIONS
6.2.2. RINSING TIP
A 0.25 mL dose of titrant will be dispensed from the burette when this operation is selected. This operation will eliminate
any contamination from the anti-diffusion dispensing tip.
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6.2.3. MANUAL DISPENSE
Option: 0.000125 to 4.750 mL (5 mL Burette)
Manual Dispense allows a defined titrant volume to be dosed. Select the Manual Dispense option and press
.
The Manual Volume Dispense screen will become active and the display will prompt you to enter the desired volume
to be dispensed.
2
6.2.4. PURGING BURETTE
This option allows the burette to be emptied before cleaning and/or storing.
INSTRUCTION MANUAL
Note: Before starting this operation, remove the aspiration tube from the titrant bottle.
The figures below show the steps in a purge burette operation.
6.3. STIRRER
Note: When custom stirrer is selected (see General Options section), the commands related to the stirrer are not
available.
In Idle mode the stirrer can be turned on and off by pressing
.
During the titration process, the stirring speed can be manually adjusted by using the
and
keys.
Note: The stirrer can not be turned off during the titration process.
To access the Data Parameters screen, press
.
From the Data Parameters screen you can access the following options:
AUXILIARY FUNCTIONS
6.4. RESULTS
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6.4.1. REVIEWING LAST REPORT
The last titration report can be reviewed.
INSTRUCTION MANUAL
2
The information seen in the report is based on the selections made in the Setup Titration Report screen.
The following option keys are available:
Review the titration graph.
Print the titration report.
Return to the previous screen.
Keys can be used to scroll through the pages.
AUXILIARY FUNCTIONS
6.4.2. REVIEWING AVAILABLE REPORTS
Up to 100 reports can be saved on the titrator. To view one of the saved reports highlight a report and then press
.
The report contains only the information selected in the Setup Titration Report screens during report generation.
The following option keys are available:
Review the selected graph.
Review the selected report.
Print the selected report.
Delete the selected report.
Return to the previous screen.
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6.4.3. GLP DATA
Option: Up to 20 characters
INSTRUCTION MANUAL
Company Name: Allows the company name to be recorded in each report.
Operator Name: Allows the operator name to be recorded in each report.
Electrode Name: Allows the electrode name to be recorded in each report.
Fields 1, 2, 3: Allows any additional information to be recorded in each report.
The fields must be selected from the Setup Titration Report screen (see Setup Titration Report) in order to be
displayed in the titration report.
6.4.4. METER INFORMATION
Displays titrator configuration data.
AUXILIARY FUNCTIONS
Titrator Serial Number:
Analog Board Serial Number:
Stirrer Serial Number:
Stirrer Software Version:
Titrator Software Version:
Base Board Software Version:
Analog Calibration Date:
Resources Version:
The serial number of the titrator base board.
The serial number of the titrator analog board.
The serial number of the stirrer.
The current software version of the stirrer.
The current software version installed on the titrator.
The current software version present on the base board of the titrator.
Manufacturer calibration date of analog board.
The current of the text resources.
Note: If more than 1 year elapsed from the calibration date of the analog board, the message Analog Calibration
Due will appear on the main screen and analog board recalibration must be performed.
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6.4.5. SETTING UP TITRATION REPORT
Customize a unique report to record the titration results. An asterisk means that it will be included in the titration report.
INSTRUCTION MANUAL
2
Adds the highlighted information to the report.
Removes the highlighted information from the report.
Returns to the Data Parameter Screen. Report is not updated.
Update the report with the select items. Report previously saved will not be updated.
Scroll through the options.
AUXILIARY FUNCTIONS
6.4.6. RESULT HISTORY
This option allows the user to access the sample analysis history and average the titration results.
Use the and keys to scroll the results list.
Use
to choose the samples that will be used for averaging.
Note: When there are no results selected, dashes will appear in the Average Sample Concentration and the Standard
Deviation fields.
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7. MAINTENANCE AND PERIPHERALS
2
7.1. BURETTE MAINTENANCE
7.1.1. BURETTE ASSEMBLY
The burette assembly consists of a rigid housing which holds the glass syringe, a 3-way valve and titrant tubing. The
burette assembly is delivered with a 5 mL syringe and with all of the accessories mounted (see Setup section).
Note: The dispensing tube has two fitted ends. One end is equipped with a burette fitting and the other is equipped
with a beaker fitting.
7.1.1.1. CHANGING THE BURETTE
Remove the burette from the pump assembly by sliding it forward and then slide the new burette into place (see the
picture below).
MAINTENANCE AND PERIPHERALS
7.1.1.2. DISASSEMBLING THE DISPENSING TUBE AND ASPIRATION TUBE
Both the aspiration and the dispensing tubes have a fitting and a tube protector. The aspiration tube will be mounted
on the left side and the dispensing tube will be mounted on the right side of the burette.
To remove the dispensing tube and the aspiration tube follow these steps:
• Remove the blue tube protector (A) by sliding it off the clear titrant tubing
• Remove the tube lock (B) from the burette holder
• Turn the fitting (C) counter-clock wise to remove it from the burette holder
• Slide the clear titrant tubing through the fitting.
INSTRUCTION MANUAL
The 5 mL burette included with the titrator exceeds the ISO 8655 standard for the accurate delivery of liquids by a
motor-driven piston burette.
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MAINTENANCE AND PERIPHERALS
INSTRUCTION MANUAL
2
7.1.1.3. ASSEMBLING THE DISPENSING TUBE AND ASPIRATION TUBE
To attach the dispensing tube and the aspiration tube follow these steps:
• Insert the flat-shaped end of the titrant tubing into the valve outlet (A) and screw the fitting clock-wise to
tighten. The highest of the 9 cuts should be vertical in the final position
• Bend the tube up into the vertical position to enter the highest cut of the fitting (C)
• Replace the tube lock fitting (D)
• Replace the blue tube protector (E) by sliding it over the clear titrant tubing, the protector will sit in the tube lock
fitting
• Repeat these steps for the aspiration tube.
7.1.1.4. CLEANING THE BURETTE
To clean the burette, follow these steps:
• If the burette is filled with titrant, remove the aspiration tube from the titrant bottle and purge burette (see
Auxiliary Functions section)
• Insert the aspiration tube into the Karl Fischer solvent
• Prime burette to fill the burette with solvent (use 2 rinses) (see Auxiliary Functions section)
• During second refilling of the burette remove the aspiration tube from the solvent or cleaning solution and allow
the air to replace the liquid in the burette.
If this simple cleaning procedure is not adequate, continue with these steps:
• Slide the burette out from the pump assembly
• Remove the dispensing and aspiration tubes. Clean them separately or use new ones
• Use HI900942 Burette Removal Tool to remove the protective cap from the bottom of the burette assembly
• Use your fingers to unscrew the syringe from the burette assembly
• Extract the piston from the syringe
• Clean both the piston and the syringe with appropriate cleaning solution
• Remove the excess liquid.
Note: R inse the tubes, syringe and piston with dry solvent (ethanol, isopropanol, or methanol) before reassembling
to remove any excess water.
Warning! Avoid contacting the titrant with bare hands. Avoid spilling titrant. Clean the external side of the syringe
and piston to remove aggressive chemicals. Do not touch the white PTFE part of the piston or internal walls
of the burette with bare hands or greasy materials.
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MAINTENANCE AND PERIPHERALS
7.1.2. BURETTE PREPARATION (TITRANT FILLING)
Before starting a titration, the burette must be properly filled with titrant in order to obtain accurate and repeatable
results. To fill the burette, follow the next steps and recommendations:
• If necessary, clean the burette and make sure it is empty
• From the main screen press
• Highlight Prime Burette option and press
• Enter the number of times the burette needs to be rinsed (a minimum of three rinses is recommended).
• Press
• Insert the aspiration tube into the titrant bottle only when the piston is going down and has reached about ¼
from the top.
• To avoid the presence of air bubbles inside the burette, ensure to have a continuous liquid flow inside the burette.
A little air just above the liquid level at the first filling is normal. The next filling will evacuate all of the air; no
air will be left in the valve.
• Sometimes during this process, slight finger tapping on the tubes is helpful to remove any residual air bubbles
from the tubes.
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INSTRUCTION MANUAL
Consult Manufacturer’s MSDS for safe handling instructions.
• Reinsert the piston into the syringe
• Use your fingers to screw the syringe into the burette assembly
• Reinsert the protective cap to the bottom of the burette assembly. Carefully position the cap into the burette
• Slide the burette into the burette stand. Position the piston shaft to couple the pump correctly
• Priming the burette three times with new titrant is recommended.
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INSTRUCTION MANUAL
2
7.2. PROBE MAINTENANCE
Proper probe maintenance is crucial for reliable measurements and extending the life of the probe. The frequency of
maintenance will depend largely on the type of samples that are analyzed. Maintenance may be required if any of the
following are observed:
• Slow or no electrode response
• Noisy mV readings
• Debris on or between electrode pins
• Coating on electrode pins
If these signs are observed, the electrode pins may be dirty. Rinse the electrode with a solvent that is appropriate for the
type of sample used – methanol is usually sufficient.
Allow the probe to dry completely before reinstalling.
If a more thorough cleaning is required, soak the electrode for several hours in HI7061 General Purpose pH Electrode
Cleaning Solution, then rinse with water followed by methanol. Allow to dry before reinstalling.
After allowing the probe to dry, inspect the glass for any cracks, especially near the electrode pins. Replace the electrode
if any cracks are found.
Warning! Take care to protect the electrode pins from damage! Avoid using brushes/abrasives to clean the pins. Pins
can easily bend, which will cause permanent errors in mV readings!
7.3. PERIPHERALS
MAINTENANCE AND PERIPHERALS
7.3.1. CONNECTING TO A PRINTER
A variety of parallel printers can be connected to the parallel port of the titrator using a DB25 cable.
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Warning! The titrator and the external printer must be both turned OFF before they are connected.
7.3.2. CONNECTING TO A COMPUTER
The titrator can be connected to a computer using a USB cable. HI900 PC application needs to be installed on the PC.
2
INSTRUCTION MANUAL
Connect the cable to the USB port on the rear panel of the titrator.
Connect the cable to the USB port on the PC.
Open the USB Link with PC screen on the titrator (see General Options section).
Launch the HI900 PC application and then select the appropriate USB Port on the PC.
Warning! Connection/disconnection of POWER CORD, PUMP ASSEMBLY, PRINTER or BALANCE must only be done
when titrator and external devices are turned off.
MAINTENANCE AND PERIPHERALS
The HI900 PC application allows the transfer of methods and reports between the titrator and PC.
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7.3.3. CONNECTING AN EXTERNAL PC KEYBOARD
This connection allows you to use an external PS/2 PC Keyboard in addition to the titrator’s keypad.
INSTRUCTION MANUAL
2
The correspondence between the titrator’s keypad and the United States 101-type external keyboard can be found
below:
External PC Keyboard (United States 101)
Titrator Keypad
Function Key F-1
Function Key F-2
MAINTENANCE AND PERIPHERALS
Function Key F-3
Function Key F-4
Function Key F-5
Function Key F-6
Function Key F-7
Function Key F-8
Function Key F-9
Option Key 1 (from left to right)
Option Key 2 (from left to right)
Option Key 3 (from left to right)
Option Key 4 (from left to right)
Option Key 5 (from left to right)
Function Key F-10
Arrow Key: Up
Arrow Key: Down
Arrow Key: Left
Arrow Key: Right
Page Up
Page Down
Numeric Keys: 0 to 9
to
Enter
Alphanumeric Keys
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Allow alphanumeric entries
8. METHOD OPTIMIZATION
2
8.1. TITRATION SETTINGS
INSTRUCTION MANUAL
The default settings included with standard methods that have been developed by Hanna Instruments in order to provide
accurate results for the majority of samples without requiring additional analyst input or method fine-tuning. However,
in order to suit a wider variety of sample types and matrices, all of the HI933 titration parameters are customizable. This
section provides the descriptions of critical titration parameters necessary for an analyst to modify a standard method or
develop a titration method from scratch.
HI933 methods can be modified and customized based on sample requirements, sample matrix and the reagent
formulation. The user changeable settings are separated into two categories: Control Parameters, which set critical
functions that determine the course of a titration and set the way in which titrations are terminated, and Method Options,
which control lesser features not directly affecting measurements and primarily allow advanced users to shorten titration
times.
8.2. CONTROL PARAMETERS
METHOD OPTIMIZATION
8.2.1. END POINT POTENTIAL AND POLARIZATION CURRENT
The HI933 uses a polarized electrode system known as bivoltametric indication. The titrator monitors the voltage
required to maintain a constant polarization current (Ipol) between the dual platinum-pin Karl Fischer electrode during
the course of a titration.
During a titration, no excess iodine is present. In order to maintain the set polarization current, the HI933 must apply a
relatively large voltage across the pins of the electrode.
At the end point of a titration, the amount of iodine added is equal to the amount of water from the sample. When an
excess of titrant has been added, iodine is present in the solution. The excess iodine is easily reduced, and the resulting
iodide is easily oxidized in electrode reactions at the cathode and anode respectively. The ease of these reactions makes
maintaining the constant polarization current possible at a much lower electrode potential.
In theory, a large shift in the electrode potential indicates the end point. In practice, a titration end point is reached when
the electrode potential drops below a predefined value and the chosen termination criteria is met.
The choice of end point potential should be based, foremost, on the polarization current and, to a lesser extent, on the
composition of the Karl Fischer solvent and the sample matrix. If the polarization current is changed, the end point
potential must also be changed. In addition, there are pitfalls to be avoided when choosing an end point potential.
Selecting end points which are both ‘too high’ or ‘too low’ will result in long titration times and poor reproducibility. End
points which are ‘too high’ are those which result in end points that either precede or coincide with equivalence point
such that the concentration of excess iodine is not reliably detected. End point potentials are considered ‘too low’ when
they correspond to a large excess of iodine in the titration cell.
Additionally, the duration of a titration is proportional to the polarization current. Thus, titration time can be reduced
by increasing the polarization current. While the default (Ipol) value of 20 μA results in a faster titration than smaller 1,
2, 5, 10, and 15 μA options, a further increase to 30 or 40 μA does not significantly shorten a titration. However, the
choice of higher polarization currents will speed contamination of the electrode and potentially degrade samples using
special solvent systems.
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INSTRUCTION MANUAL
2
8.2.1.1. DOSING PARAMETERS
The HI933 predicts the approaching end point and reduces the volumes of titrant added until the end point is reached.
This is a software controlled process known as dynamic dosing. Dynamic dosing prevents the addition of titrant beyond
the end point and provides enhanced data density in the vicinity of the end point, resulting in accurate end point
determination and faster titrations. The minimum and maximum dose volume must be set appropriately by the user for
dynamic dosing to be effective.
8.2.1.1.1. MINIMUM DOSE
Decreasing the minimum dose increases precision but lengthens titration time. The only exception is when stability time
has been selected as the termination criteria and there is a high drift rate. Under these circumstances, the minimum
dose must be large enough to maintain the end point potential by reacting all of the water due to the drift rate over
the course of the chosen time period. Increasing the minimum dose shortens titration time but reduces precision and
increases the chance of over-titration.
METHOD OPTIMIZATION
8.2.1.1.2. MAXIMUM DOSE
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The maximum dose volume should be adapted according to the formulation and concentration of the titrant. The
maximum dose volume should be set as high as possible without exceeding the reaction rate of the reagent system. The
table below provides suggested maximum doses for popular reagent systems based on their relative reaction rates. The
most effective way to optimize the maximum dose volume is to consider the titration duration and to examine the shape
of the titration curve. In the case where the maximum dose volume is too high, the iodine will be added faster than the
titration reaction rate. This excess iodine will result in a steep drop in electrode potential which will be interpreted by
the HI933 as an approaching end point. This will, in turn, result in the dynamic dosing algorithm reducing the dose
size until the excess iodine has had time to react. The reduced dose size effectively interrupts the titration and adds
considerable time to the titration duration. This way the titration will be repeatedly interrupted and the overall titration
time takes longer, even though the value of the maximum dose volume is set to large. The graph below shows an
example of a titration with a maximum dose that has been set to large.
Karl Fischer Reagent System
One-Component Systems
One-Component Systems for aldehydes and ketones
One-Component Systems formulated with pyridine
Two-Component Systems
Two-Component Systems formulated with pyridine
Maximum Dose Volume
20 to 30 μL
20 to 25 μL
15 to 20 μL
40 to 60 μL
25 to 30 μL
8.2.1.2. MAXIMUM DOSING MODE
If this option is enabled, when the mV value is greater than 150 mV from the set end point, the algorithm will always
dose the maximum value, thus reducing the titration time.
If the titration is noisy, there is a risk of over-titrating the cell.
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INSTRUCTION MANUAL
Because reaction rates are faster with two-component reagents than those observed with one-component reagents, the
maximum dose volume can be set slightly higher when using two-component systems. When the maximum dose is too
low, titration time will be extended.
8.2.1.3. TIMED INCREMENT
This setting controls the amount of time between successive titrant doses.
Setting the time increment appropriately is important to ensure that the titrant has adequate time to mix with the sample
such that the electrode measures a homogeneous solution before the titrator makes the decision on the size of the next
dose of titrant.
The value of the time increment is dependent on the reagent system being used. While the default value of 1 second is
compatible with any reagent system, titrations using two-component reagent systems can be expedited by decreasing
the time between successive doses.
8.2.1.5. SIGNAL AVERAGING
The chosen value for the signal averaging setting determines how many readings the electronics will average to produce
a single data point on the titration curve. While higher values of 3, 4, up to 10 readings reduce electrode response time,
they also result in a ‘smoother’ titration curve which may result in a faster titration (single unstable readings may cause
the dose volume to be reduced).
METHOD OPTIMIZATION
8.2.1.4. START MODE
The HI933 can be set to either normal or cautious start mode. The cautious start feature is designed to prevent the
accidental over-titration of a sample with very low water content. In cautious start mode, HI933 starts a titration using
the minimum dose size specified by the user rather than starting with half of the maximum dose size as with normal
start mode.
8.2.1.6. FLOW RATE
The flow rate setting specifies the volume of titrant delivered per minute. The default flow rate should be used for the
majority of titrations. In cases where the titrant is more viscous, the flow rate can be reduced.
8.2.2. TERMINATION PARAMETERS
The HI933 provides a choice of three criteria by which a titration can be considered to have successfully reached an end
point.
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METHOD OPTIMIZATION
INSTRUCTION MANUAL
2
8.2.2.1. STABILITY TIME
When this termination criteria is selected, a titration is considered to have reached an end point when the electrode
potential stays below the specified end point potential for a period of time called the stability time. Typical end point
stability times range between 5 and 15 seconds.
In order for this criteria to successfully terminate a titration the stability time and the minimum dose size must be set
such that, at the end of a titration, the minimum dose size is large enough to react all of the water leaking into the cell
due to drift during the set stability time. If the minimum dose volume is too small to compensate for the water introduced
by the drift, the titration will never be terminated.
8.2.2.2. DRIFT STOP TERMINATION CRITERIA
Drift-based termination criteria, or Drift stop, terminates titrations based on the concept that at the end of a titration,
when all of the water due to the sample has been reacted, the titrator should only be titrating the water seeping into the
cell due to the background drift rate (see Drift Analysis section for a detailed explanation of background drift).
Ideally, drift stop termination criteria would end a titration when a drift rate, identical to that which preceded the start
of a titration, is observed at the end of a titration. However, from a practical standpoint, the achievement of an identical
drift rate results in very long titration times.
In order to shorten titration times while still taking advantage of the positive aspects of drift-based termination, the
HI933 incorporates two drift stop termination criteria, relative drift stop and absolute drift stop.
8.2.2.2.1. RELATIVE DRIFT STOP
The relative drift stop termination parameter should be the first choice termination criteria. It is the most universally
applicable, easiest to use and results in fast, repeatable titrations.
This parameter has the advantage over other termination criteria in that the relative drift rate termination value can be
set independently from the titrant concentration and the initial drift rate.
Under this criteria a titration reaches an end point successfully when the HI933 titrates all of the water introduced with
the sample and maintains a drift rate which is equal to the sum of the initial drift (drift rate when the titration was
initiated) and the set ‘relative drift stop’ value (i.e. a slightly higher drift than the initial drift rate).
The choice of relative drift stop value influences the titration duration and reproducibility. Choosing low relative drift stop
values (5 to 10 μg/min) will result in titrations with high reproducibly and long durations. Setting high relative drift stop
values (20 to 30 μg/min) will result in fast titrations with potentially reduced reproducibility. Reduced reproducibility
at higher drift stop values is of particular concern when using reagents that have slower reaction rates (one-component
or aldehyde and ketone reagents).
It is important to set an appropriate relative drift stop value when working with insoluble or sparingly soluble samples.
During these types of titrations, the final traces of water are released very slowly. If the sample contains a small amount
of water (the final traces are a large fraction of the total water), the relative drift stop value should be set very low. If the
final traces can be ignored because the sample water content is large, then the titrations can be terminated at a higher
drift rate termination value.
8.2.2.2.2. ABSOLUTE DRIFT STOP
Under this criteria, a titration reaches an end point successfully when the drift falls below a predefined threshold called
the absolute drift stop value.
The absolute drift stop value does not take the initial drift rate into account but does have the advantage of being able
to be set without consideration of the titrant concentration. In addition, for a titration to reach end point, the absolute
drift stop threshold must be set higher than the initial drift rate value.
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8.2.3. METHOD OPTIONS
8.2.3.1. PRE-DISPENSING AMOUNT
It is possible to shorten titration times by adding a large fraction of the titrant at the start of the analysis if the
approximate water content of the sample is known.
When activated, the pre-dispensing amount can be set to deliver between 1% and 90% of the titrant required to reach
the titration end point. A high pre-dispensing amount (around 90%) increases the chances of erroneous results. Predispensing amounts above 50% should only be used if the reaction is very rapid.
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INSTRUCTION MANUAL
The primary disadvantage associated with the absolute drift rate termination criteria is that the actual background drift
rate must be considered before setting the absolute drift rate threshold. When setting the absolute drift threshold, a
balance must be struck between the titration speed and accuracy. Choosing a threshold slightly higher than the initial
drift rate will result in high reproducibility and relatively slow titrations. Setting the threshold higher (>30 μg/min)
will result in very fast titrations and reduced titration reproducibility.
8.2.3.2. PRE-ANALYSIS STIR TIME
When analyzing solid samples with limited solubility or samples that release bound water slowly, the sample must be
stirred in the chosen solvent prior to the start of a titration, to avoid erroneously low titration results or unreachable
end points. The pre-analysis stir time option ensures that after the sample is added the titration mixture is stirred for a
period of time before any titrant is added to the cell. The pre-analysis stir time can be set between 0 and 1000 seconds.
8.2.3.4. BACKGROUND DRIFT RATE ENTRY
This option provides a choice between the HI933’s automatic drift rate determination and assigning a fixed value to be
used by the titrator as the drift rate.
The primary benefit of bypassing the automatic drift rate feature is saving time. This is appropriate when titrating
samples with high water content where the drift rate is too low to affect titration results or in diagnostic situations where
there is no advantage in waiting for the HI933 to conduct a drift rate analysis.
METHOD OPTIMIZATION
8.2.3.3. STIRRING SPEED
The HI933’s stirring speed can be set between 200 and 2000 RPM with 100 RPM resolution. The stirring system is
equipped with an optical feedback mechanism to ensure that the stirring motor is rotating at the speed set by the user.
The optimum stirring speed is obtained when a small vortex is visible. If the stirring speed is too low, the titrant will not
react with the sample before reaching the electrode resulting in over-titration and poor titration reproducibility. If the
stirring speed is too high, bubbles will form in the solution. Bubbles can destabilize or falsify the measured electrode
potential.
The default stirring speed for commercially available standard Karl Fischer reagents, used within the operable volume
range of the standard Hanna Instruments cell and with the supplied magnetic stirring bar, is 900 RPM. Samples which
result in a titration solution with higher or lower viscosity may require stir speed adjustment.
8.3. THE SAMPLE
8.3.1. PROPER SAMPLING PROCEDURE
Proper sampling is essential for accurately determining the water content of bulk materials, particularly with nonhomogeneous samples. Many standard methods detail instructions to ensure proper sampling. As a general rule, the
following guidelines should be followed:
• The sample must be representative. The water content of the sample taken is the same as the average water
content of the bulk material.
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METHOD OPTIMIZATION
INSTRUCTION MANUAL
2
• Avoid exposing samples to the contaminating effects of atmospheric moisture. Take samples as quickly as
possible and protect the sample during transport and/or storage.
• Take samples from the interior of bulk materials. Surfaces of hygroscopic materials may contain higher levels of
moisture relative to the rest of the material. Surfaces of materials which release water may contain less water
relative to the rest of the material.
• Taking large samples of bulk materials will result in a more representative sample.
8.3.2. DETERMINING THE OPTIMAL SAMPLE SIZE
The proper choice of sample size is critical to achieving accurate and repeatable titration results. As a general rule, the
sample size should be selected such that about 30-70% of the burette volume is consumed during a titration. This
provides enough titrant to ensure good accuracy while conserving reagents and minimizing the generation of waste.
The table below illustrates the relationship between titration reproducibility, the volume of titrant consumed during a
titration, the amount of water contained in a sample, the size of a sample and the water content of a sample.
The ideal sample size can be estimated using the table by drawing a line from the expected water content to the amount
of water in the sample corresponding to the desired titration reproducibility (relative standard deviation). The ideal
sample size is indicated by where the drawn line intersects the ‘size of sample’ scale.
Consider the line on the table as an example. The line was drawn for a user with a sample having approximately 1%
water who required the best possible reproducibility. The intersection of the red line with the size of sample column
indicates that in order to introduce the optimal 10 mg of water into the titration cell, the user must add 1g of sample.
The amount of sample required to introduce 10 mg of water into the titration cell can also be calculated directly using
the equation below.
Sample mass (g ) =
1
%H 20 in sample
8.3.3. SOLID SAMPLES
Sample water must be available to react with the titrant. This typically means that the sample must be adequately
dissolved in the solvent. This is achieved by choosing an appropriate solvent system, proper preparation of the sample
and optimization of the reaction conditions. After ensuring that the sample is soluble in the choice of solvent or solvent
mixture, dissolution of a solid sample can be aided by grinding the sample into a fine powder, increasing the preanalysis stir time or heating the solvent during a titration with an optional jacketed titration cell and water circulator.
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METHOD OPTIMIZATION
8.3.4. LIQUID SAMPLES
As with solids, the water contained in liquid samples must be available to react with the titrant. It is important to select
a solvent system or mixture with which the sample is miscible.
Liquids are typically added through the septum in the sample port via a syringe and needle using the following steps:
• Attach a long needle (approximately 6 cm long, 21-gauge) to a syringe large enough to hold at least one
complete sample volume.
• Rinse the syringe and needle with sample several times by drawing in a small portion of sample, fully extending
the plunger, shaking to coat the syringe interior and expelling the sample into a waste collection container.
• Draw enough sample into the syringe for at least one titration.
• Dry the outside of the needle with a lint free wipe or tissue.
• Determine the mass of the syringe and sample.
• Initiate a titration from standby mode by pressing the “start analysis” option key.
• Insert the needle through the septum in the sample port. Push the syringe through the septum until the end of
the needle is approximately 1 cm from the surface of the solvent.
• Steadily dispense the contents of the syringe ensuring that the sample is introduced directly into the solvent and
does not splash or spatter onto the wall of the titration vessel electrode or dispensing tip.
• Draw a small amount of air from inside the cell into the syringe to ensure that no sample drops remain on the
tip of the needle.
• Remove the syringe and needle from the septum taking care to not touch the needle to the solvent or other
internal cell components.
2
INSTRUCTION MANUAL
Solid samples are added to the titration cell by removing the sample plug. The quantity of solid sample added can be
entered into the HI933 as a mass or by number of pieces if, for example, pills are to be analyzed. The most accurate way
to determine the mass of the sample added to the cell can be achieved by an analytical technique called back-weighing.
Back-weighing consists of the following steps:
• Measure the mass of a sample in a weigh boat.
• Initiate the titration sequence on the HI933 using the ‘start analysis’ option key from standby mode. This will
bring up the “add sample” screen.
• Slide the sample plug up, out of the vessel top to open the sample port.
• Rapidly add the sample through the sample port ensuring that ALL of the sample is transferred to the solvent.
Avoid any contact between the sample and the cell walls or top.
• Replace the sample plug into the vessel top.
• Determine the mass of the “empty” weight boat.
• Calculate the mass of the sample added (subtract the mass of the emptied weigh boat from the mass of the full
weigh boat).
• Enter the calculated mass of the sample into the HI933.
• Start titration using the option key ‘start analysis’ from the add sample screen.
Care should be taken to add a solid sample as fast as possible in order to minimize the amount of time that the sample
port is open. It is also important to be sure that all of the sample reaches the solvent and does not make contact with,
or stick to, the inner sides of the vessel cap. Losing even a small fraction of the sample mass will result in a high sample
water content.
In some cases solid samples may require one of the additional preparatory steps listed in the sections that follow.
Specific sample preparation instructions are included with each standard method.
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INSTRUCTION MANUAL
2
• Determine the mass of the syringe and needle.
• Calculate the mass of the sample added to the titration cell (subtract the mass of the syringe after the sample
has been added from the mass of the syringe before sample addition).
• Enter the calculated mass of the sample into the HI933.
• Start titration using the option key
from the add sample screen.
As indicated above, when adding a liquid sample with a needle and syringe, it is important that the sample is introduced
directly into the solvent. Sample that is deposited on the sides of the vessel or other internal components of the cell
may not be titrated with the rest of the sample. It is equally important that no drops remain on the tip of the needle.
“Hanging drops” will end up on the bottom of the septum. This will result in false low results for the determination.
Liquid samples with high viscosity, like honey, can be added via a syringe without needle through the sample port
following the steps outlined above.
In some cases, liquid samples may require one of the additional preparatory steps listed in the sections that follow.
Specific sample preparation instructions are included with each standard method.
METHOD OPTIMIZATION
8.3.5. SAMPLE PREPARATION TECHNIQUES
While many samples can be introduced directly into the titration vessel (see Sample Addition section), others require
preparatory steps. It is critical that samples are not contaminated with additional water or lose water during the
preparation phase.
The steps required for the most common sample preparation techniques are outlined below. For detailed applicationspecific instructions, consult the instructions included with applicable standard methods.
The HI933 provides options for the automatic calculation of samples prepared normally, using external extraction and
external dissolution.
8.3.5.1. INTERNAL EXTRACTIONS
Internal extractions are carried out using the “normal” sample type option within the “sample parameters menu”.
This type of sample preparation is suitable for solid samples which release their water relatively quickly (during the
pre-analysis stir time) and exhibit limited or no solubility in Karl Fischer solvents. Internal extraction should be used
preferentially over external extraction techniques because the extracted water is titrated immediately, which favors
complete extraction by Le Chatlier’s principle.
An outline of the general procedure follows:
• Add methanol or an appropriate solvent to the titration cell and pre-titrate to dryness.
• Adjust the pre-analysis stir time to be sufficiently long to complete the extraction. Appropriate set times will be
sample and solvent specific. Consult an applicable standard method or experiment by increasing the pre-analysis
stir time and titrating samples until the resulting water content no longer increases.
• Reduce the samples to as fine of a powder as possible to ensure that sample water is extracted quickly.
• Add the sample to the titration vessel using the back weighing method.
8.3.5.2. DILUTIONS
It is very difficult to accurately add very small amounts of sample to the titration vessel. In order to produce accurate
and reproducible results, samples having water content greater than 50% should therefore be diluted with a dry solvent
before being introduced into the titration vessel. Dilutions are carried out using the ‘external dissolution’ sample type
option.
Anhydrous methanol is the solvent of choice for sample dilutions. If the sample contains fats or oils, then a mixture of
methanol and chloroform can be used to promote solubility of the sample.
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8.3.5.3. EXTERNAL DISSOLUTION
External dissolutions are recommended for titrations which require a large amount of soluble solid sample due to
inhomogeneous water distribution or very low water content. External dissolution reduces the error typically associated
with the titration of low water content solids by collecting the water released by a large amount of solid sample by
dissolving it in a relatively small amount of solvent. A small portion of the solvent can then be injected into the titration
vessel.
Sample preparation and choice of solvent or solvent mixture is sample specific. Consult an applicable standard method
for procedural details.
The HI933 will conduct the necessary calculations automatically when “external dissolution” is selected from the sample
type menu.
METHOD OPTIMIZATION
8.3.5.4. EXTERNAL EXTRACTION
External extraction is recommended for insoluble solid samples which release water slowly.
The HI933 will conduct the necessary calculations automatically when “external extraction” is selected from the sample
type menu.
An outline of a general procedure follows:
• Determine the mass of an extraction bottle or flask equipped with a septum.
• Add the extraction solvent to the bottle and determine the mass of the bottle and the solvent. In order to
maximize the effectiveness of the extraction, the water content of the solvent should be as low as possible. When
choosing an extraction solvent, one must carefully consider the limit of water saturation for a possible solvent.
• Determine the water content of the solvent.
• Determine the mass of the solvent remaining in the extraction bottle.
• Add a finely crushed sample to the solvent in the extraction bottle. The amount of sample added should be large
enough so that the amount of water in the sample is much greater than that in the solvent before the extraction.
• Facilitate extraction by shaking the solution or placing the solution on a stirring plate or in a sonicator.
• Allow the insoluble portion of the sample to settle to the bottom of the extraction bottle.
• Titrate an appropriately sized sample of the supernatant (solvent above the settled solid sample).
2
INSTRUCTION MANUAL
The following outlines a generic dilution procedure:
• Determine the mass of a dry flask equipped with a septum stopper.
• Transfer approximately 1 g of sample to the flask and measure the mass of the flask and the sample together.
• Add 30 grams of dilution solvent to the flask. Re-seal and mix the flask contents.
• Determine the moisture content of the dry solvent used as the diluent in a separate titration.
• Add the diluted sample as per the instructions for adding liquid samples in this section.
8.3.5.5. HOMOGENIZATION
Homogenization is recommended for non-aqueous or mixed phase liquid samples as well as solids with inhomogeneous
distributions of water. Water can be evenly distributed throughout a collected sample by the use of high speed, high
shear mixers called homogenizers.
In mixed phase (oil and water) non-aqueous samples, water tends to migrate to the surface of the sample solution,
adhere to the inner walls of or sink to the bottom of the sample bottle. This is particularly problematic when sampling
is done at high temperatures and the specimen is subsequently allowed to cool to room temperature prior to analysis.
Solid samples typically exhibit inhomogeneous water distributions and must therefore be thoroughly reduced to powder
or homogenized. The procedure for homogenization depends upon the characteristics of the specific sample.
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INSTRUCTION MANUAL
2
Homogenization is particularly suited for semi-solid samples and suspensions and is the only method that can disrupt
plant and tissue cells in order to release water present inside the cells. Homogenization is typically carried out externally
in a dry flask with the addition of a suitable solvent, preferably methanol.
8.3.5.6. HEATING
Sample heating is used for the analysis of solid or liquid samples that cannot be extracted or that interfere with the Karl
Fischer reaction. These include plastics, minerals, petrochemical products which contain additives, and starting materials
for pharmaceutical products.
Samples are heated in a special oven while a dry stream of carrier gas passes through the sample chamber or, for liquid
samples, the sample itself. The carrier gas is introduced into the titration vessel.
The heating temperature is sample specific and can be found in applicable standard methods. The temperatures are
chosen to be as high as possible without decomposing the sample, which can result in contamination of the titration
vessel.
8.4. KARL FISCHER REAGENT SYSTEM
METHOD OPTIMIZATION
A wide variety of Karl Fischer reagents exist on the market today, each designed and formulated for specific sample
matrices and titration conditions. Karl Fischer reagent systems consist of a solvent and a titrant. The solvent is the liquid
to which the sample is added in the reaction vessel. The titrant is the iodine-containing liquid pumped into the cell
during the titration.
8.4.1. REAGENT SYSTEM CLASSIFICATION
Reagent systems are classified as either one-component or two-component depending on whether the sulfur dioxide and
base are included in the titrant or with the solvent. In one-component systems, also known as composites, the titrant
contains all of the reactants needed to conduct the titration (iodine, sulfur dioxide and a base) dissolved in an alcohol or
ether. In a two-component reagent system, the solvent already contains the sulfur dioxide and the base while the titrant
is typically a solution consisting of iodine and methanol.
8.4.1.1. ONE-COMPONENT REAGENT SYSTEMS
One-component reagents are less stable than two-component systems, typically having only a two-year shelf life, but
they provide several significant advantages. The major advantage is that the titrant is providing the sulfur dioxide and
the base. The constant supply of reaction components from the titrant allows a high level of flexibility with respect to the
chemical composition of the solvent and provides a nearly limitless solvent capacity for water. One-component solvent
systems can be easily customized, creating mixtures specially adapted to specific sample characteristics without having
to worry about providing appropriate levels of sulfur dioxide and buffer components. Common solvent mixtures include
ethanol, chloroform, xylene, toluene, and long chain alcohols such as hexanol and decanol.
8.4.1.2. TWO-COMPONENT REAGENT SYSTEMS
Two-component reagents have advantages of their own. They are more stable and have a longer shelf life than onecomponent systems. The sulfur dioxide is pre-mixed in excess with an alcohol-based solvent, therefore the necessary
reactive sulfite esters are present in vast excess prior to the start of a titration. This results in higher titration speeds and
greater accuracy for low levels of water. In addition, having the base present in excess in the solvent prior to sample
addition results in a higher solvent buffer capacity.
8.4.1.3. REAGENTS FOR ALDEHYDES AND KETONES
The addition of a sample containing aldehydes or ketones to a methanol-based Karl Fischer solvent results in side
reactions that adversely affect titration results. When alcohols react with the carbonyl groups of aldehydes and ketones
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8.4.2. CHOOSING AND MODIFYING A SOLVENT
The solvent plays an important role in the KF titration. It must react with sulfur dioxide to form the reactive methyl sulfite
species, dissolve the sample and/or extract water, and it should help prevent side reactions from occurring. The most
common solvent is methanol. Co-solvents can be added to increase sample solubility in one-component solvents, as
long as the mixture contains at least 20 - 30% methanol. In a two-component reagent system, 50% solvent for twocomponent system and 50% co-solvent can be used. This ensures that there is enough sulfur dioxide and base for the
Karl Fischer reaction to take place.
In general, a solvent should be chosen in accordance with the sample composition.
Fats, oils and long-chain hydrocarbons have limited solubility in methanol. Co-solvents of long-chain alcohols
(n-decanol) or chloroform should be used.
Carbohydrates and proteins have poor solubility in methanol, formamide can be used as a co-solvent. Analyzing acids or
bases may take the pH outside the optimal range and additional buffering may be required. A commercial Karl Fischer
‘Buffer’ reagent can be added or extra imidazole for acid samples and salicylic acid to the solvent for basic samples
For analysis of ketones or aldehydes, the methanol can be replaced with special “K” reagents that contain mixtures
including 2-chloroethanol, chloroform, ethanol or 1-methoxy-2-propanol.
METHOD OPTIMIZATION
8.4.3. WATER STANDARDS
Water standards are used to standardize the titrant and to verify the titrator’s performance and analyst technique. Water
standards are an integral part of ISO 9000, GMP, GLP and FDA guidelines for water determination.
The most commonly utilized water standard for volumetric Karl Fischer titration is sodium tartrate dihydrate. Available as
a highly-purified, non-hygroscopic powder, sodium tartrate dihydrate has a stable water content of 15.66 ± 0.05%.
The compound is, however, sparingly soluble in methanol requiring at least 3 minutes of stirring for complete dissolution.
If high precision or NIST traceability is required, water standards sealed in glass ampules are also commercially
available. Although they are more expensive, sealed standards come pre-analyzed and certified by the manufacturer
and are available in a wide range of concentrations.
The experienced analyst can also use very small volumes of deionized water as a standard. Due to the very watersensitive nature of a Karl Fischer titration, only a few milligrams of water are required for a typical standardization or
system verification. A great deal of skill is therefore required in determining the mass of the water introduced into the
titration vessel in order to achieve highly accurate results.
2
INSTRUCTION MANUAL
they form acetals and ketals via a reaction that releases water. The generation of water during a titration will falsely
inflate water content results and could lead to vanishing end points.
While ketones are less reactive than aldehydes, the reactivity of both species is inversely proportional to carbonyl chain
lengths. The formation of acetals and ketals is also dependent on the type of alcohol included in the solvent. As the chain
length of an alcohol’s alkyl or substituted alkyl group increases, the alcohol’s reactivity toward ketones and aldehydes
decreases (i.e. methanol is the most reactive). Acetal or ketal formation can be prevented by the use of methanol-free
reagents specially produced for this purpose. Reagents for aldehyde and ketone analysis replace methanol with higher
alcohols, ethers, halogenated alkanes or similar combinations.
8.4.4. STANDARDIZING THE TITRANT
Standardizing the Titrant, or determining the titer, is a routine and necessary part of accurate Karl Fischer analyses.
The titrant should be standardized daily for greatest accuracy. Standardization serves to standardize the combination of
parameters selected as part of a particular method and serves as a system check. It is recommended that the titrant be
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METHOD OPTIMIZATION
INSTRUCTION MANUAL
2
2-94
re-standardized if the method to be used for an analysis is very different from that which was used to standardize the
titrant initially. The titrant can be standardized using hydrated salt, liquid water standards or tiny amounts of pure water.
A general procedure for titrant standardization is detailed below.
• Setup titrator according to the instruction manual. Ensure the titrator is set up with the same reagents, solvents,
working conditions, temperature and titrator settings to be used for subsequent sample analyses.
• Select the appropriate standardization method included with the HI933.
If using a Sodium Tartrate Dihydrate Standard:
• Back-weigh between 30 and 200 mg of standard. Be sure that the salt is a high quality standard, which has
been stored properly and exists as a fine, free flowing powder.
• Repeat the standardization at least three times and update the titrant concentration using the averaged result
value via the statistics screen if the variability between the standardizations is small.
If using a Prepared Liquid Water Standard (Ampule):
• Break open an ampule of standard. Rinse a syringe with a small portion of standard.
• Draw up the remainder of the standard into the syringe, weight and titrate about one third of the standard in
the syringe.
• Conduct two more standardizations with the standard remaining in the syringe.
• Review the set of results on the “average results” statistics screen. The titrant concentration should be updated
with the averaged results as long as there is not excessive variability between standardization results.
If using pure water standards:
• Draw approximately 10 μL of pure water into a glass micro-liter syringe.
• Introduce the water standard by back-weighing using an analytical balance with 0.01 mg resolution. Because of
the extremely small sample size, it is important to strictly follow the procedure for the addition of liquid samples
outlined in the section “Liquid samples” above.
• Review the set of results on the “average results” statistics screen. The titrant concentration should be updated
with the averaged results as long as there is not excessive variability between standardization results.
9. ACCESSORIES
2
9.1. TITRANTS
9.2. SOLVENTS
ACCESSORIES
9.1.4.3.2. TWO-COMPONENT TITRANTS
Honeywell®
HYDRANAL™ - Titrant 2 (Catalog Number 34811)
HYDRANAL™ - Titrant 2 E (Catalog Number 34723)
HYDRANAL™ - Titrant 5 (Catalog Number 34801)
HYDRANAL™ - Titrant 5 E (Catalog Number 34732)
GFS Chemicals® Watermark® - Non-hygroscopic Titrant, 0.5 mg/mL (Catalog Number 1970)
Watermark® - Non-hygroscopic Titrant, 1 mg/mL (Catalog Number 1602)
Watermark® - Non-hygroscopic Titrant, 2 mg/mL (Catalog Number 1603)
Watermark® - Non-hygroscopic Titrant, 5 mg/mL (Catalog Number 1604)
J.T. Baker®
Hydra-Point™ - Composite 2 (Catalog Number 8845)
Hydra-Point™ - Composite 5 (Catalog Number 8844)
INSTRUCTION MANUAL
9.1.4.3.1. ONE-COMPONENT TITRANTS
Honeywell®
HYDRANAL™ - Composite 1 (Catalog Number 34827)
HYDRANAL™ - Composite 2 (Catalog Number 34806)
HYDRANAL™ - Composite 5 (Catalog Number 34805)
HYDRANAL™ - Composite 5 K (Catalog Number 34816)
®
GFS Chemicals Watermark® - Single Solution, 2 mg/mL (Catalog Number 1601)
Watermark® - Non-Hazardous Single Solution, 2 mg/mL (Catalog Number 1894)
Watermark® - Single Solution, 5 mg/mL (Catalog Number 1600)
Watermark® - Non-Hazardous Single Solution, 5 mg/mL (Catalog Number 1893)
Watermark® - Methanol Based, 5 mg/mL (Catalog Number 1616)
J.T. Baker®
Hydra-Point™ - Composite 2 (Catalog Number 8891)
Hydra-Point™ - Composite 5 (Catalog Number 8890)
Hydra-Point™ - Composite 5K (Catalog Number 8892)
9.2.4.3.1. ONE-COMPONENT SOLVENTS
Honeywell®
HYDRANAL™ - Methanol Dry (Catalog Number 34741)
HYDRANAL™ - Methanol Rapid (Catalog Number 37817)
HYDRANAL™ - CompoSolver E (Catalog Number 34734)
HYDRANAL™ - Solver (Crude) Oil (Catalog Number 34697)
HYDRANAL™ - LipoSolver CM (Catalog Number 37855)
HYDRANAL™ - LipoSolver MH (Catalog Number 37856)
HYDRANAL™ - Medium K (Catalog Number 34698)
HYDRANAL™ - KetoSolver (Catalog Number 34738)
HYDRANAL™ - Working Medium K (Catalog Number 34817)
HYDRANAL™ - Karl Fischer Reagent (Catalog Number 36115)
2-95
INSTRUCTION MANUAL
2
GFS Chemicals® Watermark® - General Purpose Solvent (Catalog Number 1610)
Watermark® - Methanol Solvent (Catalog Number 1609)
Watermark® - Ketone/Aldehyde Solvent (Catalog Number 5322)
Watermark® - Oils Solvent (Catalog Number 2978)
Watermark® - Methyl Alcohol - KF Grade (Catalog Number 3569)
J T Baker®
Hydra-Point™ - Methanol Dry (Catalog Number 8898)w
9.2.4.3.2. TWO-COMPONENT SOLVENTS
Honeywell
HYDRANAL™ - Solvent (Catalog Number 34800)
HYDRANAL™ - Solvent E (Catalog Number 34730)
HYDRANAL™ - Solvent CM (Catalog Number 34812)
HYDRANAL™ - Solvent Oil (Catalog Number 34749)
®
GFS Chemicals Watermark® - General Purpose Solvent (Catalog Number 1610)
Watermark® - Methanol Free Solvent (Catalog Number 1609)
Watermark® - Buffer (Catalog Number 1615)
Watermark® - KF Solvent for Oil (Catalog Number 2991)
J.T. Baker®
Hydra-Point™ - Solvent G (Catalog Number 8855)
9.3. STANDARDS
Honeywell®
ACCESSORIES
GFS Chemicals®
2-96
HYDRANAL™ - Standard Sodium Tartrate Dihydrate (Catalog Number 34696)
HYDRANAL™ - Water Standard 10.0 (Catalog Number 34849)
HYDRANAL™ - Water Standard 1.0 (Catalog Number 34828)
HYDRANAL™ - Water Standard 0.1 (Catalog Number 34847)
Watermark® - Sodium Tartrate (Catalog Number 805)
Watermark® - 10 mg/g (Catalog Number 2303)
Watermark® - 5.00 mg/g (Catalog Number 2304)
Watermark® - 1.00 mg/g (Catalog Number 2302)
Watermark® - 0.50 mg/g (Catalog Number 3493)
Watermark® - 0.100 mg/g (Catalog Number 2301)
Watermark® - 0.050 mg/g (Catalog Number 2311)
2
9.4. TITRATOR COMPONENTS
INSTRUCTION MANUAL
Pump Assembly
HI930100
Aspiration Tubing
HI900570S
Dispensing Tubing
and Fitting
HI900580S
Beaker Assembly
HI930520
5 mL Burette Assembly
HI930505
ACCESSORIES
Tool for Burette Cap
Removal
HI900942
Air Pump and magnetic
stirrer for HI933/HI934
HI930180
Dispensing Tip (2 pcs.)
HI900523
Beaker for HI903/HI933
HI900522
Solvent Port Plugs (2 pcs.)
HI900528
5 mL Syringe
HI900205
2-97
ACCESSORIES
INSTRUCTION MANUAL
2
2-98
Titrant Bottle Top Assembly
HI900530
Septum (5 pcs.)
HI900527
Solvent/Waste Bottle Top
Assembly
HI900531
Desiccant, 250 g
HI900550
Desiccant Cartridge for
Titration Beaker or Titrant
Bottle
HI900532
Power Adapter (USA Plug)
HI900946
Desiccant Cartridge for
Solvent or Waste Bottle
HI900533
Power Adapter (European Plug)
HI900947
Waste Bottle
HI900534
Calibration Key
HI900941
Tubing for Solvent/Waste
Handling (2 pcs.)
HI900535
USB Cable
HI920013
Tubing for Air Pump (2 pcs.)
HI900536
USB Flash Drive
HI930900U
O-Ring Set
HI900540
Instruction Manual Binder
HI930803
PART 3:
APPLICATIONS
APPLICATIONS
3

3
HI8001EN 5.0 mg/mL TITRANT STANDARDIZATION WITH WATER STANDARD
HI8001EN
APPLICATIONS
One-Component Titrant
3-2
DESCRIPTION
Method for the standardization (titer determination) of 5.0
mg/mL one-component Karl Fischer titrant using a Liquid
Water Standard. The results are expressed in mg/mL.
ELECTRODE
• HI76320 Dual Platinum Pin Electrode
REAGENTS
• 5 mg/mL one-component Karl Fischer volumetric
titrant
• 10 mg/g Liquid water standard
• Dry methanol
ACCESSORIES
• 3 mL syringe (clean and dry)
• 22-gauge, 6” non-coring septum penetration needle
(clean and dry)
• Solvent bottle, GL45 thread
DEVICE PREPARATION
• Connect the solvent bottle top assembly to the bottle
of methanol according to the manual.
• Assemble the titration vessel according to the
instruction manual.
• Install a 5 mL burette filled with 5 mg/mL onecomponent Karl Fischer volumetric titrant to be
standardized and verify that no air bubbles are
present in the burette or tubing. If necessary, prime
until all air has been removed completely.
• Press
from the main screen. Use the arrow
keys to highlight HI8001EN 5mg/mL Stdz w/water
std and press
.
• Dispense enough methanol from the solvent bottle
to fill the vessel to the “min” line (about 50 mL).
• Press
to pre-titrate the solvent and the titration
vessel moisture. Allow the background drift rate to
stabilize before proceeding to the next step.
ANALYSIS
• Fill the syringe and needle with the water standard.
• Weigh the syringe, needle and water standard.
• Press
. You will be prompted to enter the
sample size.
• Dispense 1.00 g (about 1 mL) of standard into the
titration vessel through the septum using the needle.
• Pay attention not to get any sample on the electrode
or beaker wall. If necessary, swirl the titration vessel
gently by hand to remove any standard from the
electrode or beaker wall.
• Clear the needle of residual standard by intaking a
small volume of air from the titration vessel. If a
“hanging drop” of standard is seen on the end of
the needle, dip the end of the needle briefly in the
solvent.
• Remove the needle from the titration vessel and
weigh the syringe again in order to determine the
exact amount of standard added (by difference of
the two measurements.)
• Use the numeric keypad to enter the exact weight
and press
to start the analysis.
• At the end of the titration, the Standardization
Result screen is displayed. The results are expressed
in mg/mL.
CALCULATIONS
Name:
5mg/mL Stdz w/water std
Method Revision:
1.1
Type:
Titrant Standardization
Predispensing Amount:
25 %
Pre-Analysis Stir Time:
5 Sec
Stirring Speed:
900 RPM
Stirbar Type:
Medium
Drift Entry:
Automatic
Solvent:
Methanol
Standard:
Liquid 10 mg/g
Type:
Liquid by mass
Concentration Unit:
mg/g
Water Content:
10.0000 mg/g
Standard Size:
1.0000 g
Titrant:
Composite 5
Titrant Type:
one-component
Nominal Titrant Conc.: 5.0000 mg/mL
Std. Titrant Conc.:
5.0000 mg/mL
Date/Time:
Apr 02, 2019 11:45
Titrant Age Reminder:
2d:00h:00m
Control Parameters:
Start Mode:
Normal
Standby Mode:
Enabled
Standby Duration:
12:00 [hh:mm]
Imposed Current:
20 μA
Minimum Dose:
0.500 μL
Maximum Dose:
20.000 μL
Max Dosing Mode
Disabled
Timed Increment:
1 second
End Point Value:
180.0 mV
Signal Averaging:
3 Readings
Flow Rate:
10.0 mL/min
Termination Parameters:
Maximum Duration:
1200 sec
Maximum Titrant Volume: 10.000 mL
Term. Criterion:
Relative Drift
Relative Drift:
7.0 μg/min
Significant Figures
XXXXX
Titrant units:
mg/mL
Titrant volume consumed:
V (mL)
Final Results Units:
mg/mL
Standard Concentration: 10.0000 mg/g
Standard mass:
1.0000 g [w/w]
RESULTS
3
APPLICATIONS
METHOD PARAMETERS
Titration Report
Method Name: 5mg/mL Stdz w/water std
Time & Date:
Apr 03, 2019 12:00
Standard Size:
1.0000 g
Standard Conc.:
10.0000 mg/g
Drift Value:
5.4 μg/min
End Point Volume:
2.0341 mL
Result:
4.9276 mg/mL
Titration Duration:
4:19 [mm:ss]
Estimated Cell Volume:
55.88 mL
Titration went to Completion
Operator Name:
Analyst Signature:__________________
HI8001EN
3-3
3
HI8002EN 2.0 mg/mL TITRANT STANDARDIZATION WITH WATER STANDARD
HI8002EN
APPLICATIONS
One-Component Titrant
3-4
DESCRIPTION
Method for the standardization (titer determination) of 2.0
mg/mL one-component Karl Fischer titrant using a Liquid
Water Standard. The results are expressed in mg/mL.
ELECTRODE
• HI76320 Dual Platinum Pin Electrode
REAGENTS
• 2 mg/mL one-component Karl Fischer volumetric
titrant
• 1 mg/g Liquid water standard
• Dry methanol
ACCESSORIES
• 3 mL syringe (clean and dry)
• 22-gauge, 6” non-coring septum penetration needle
(clean and dry)
• Solvent bottle, GL45 thread
DEVICE PREPARATION
• Connect the solvent bottle top assembly to the bottle
of methanol according to the manual.
• Assemble the titration vessel according to the
instruction manual.
• Install a 5 mL burette filled with 2 mg/mL onecomponent Karl Fischer volumetric titrant to be
standardized and verify that no air bubbles are
present in the burette or tubing. If necessary, prime
until all air has been removed completely.
• Press
from the main screen. Use the arrow
keys to highlight HI8002EN 2mg/mL Stdz w/water
std and press
.
• Dispense enough methanol from the solvent bottle
to fill the vessel to the “min” line (about 50 mL).
• Press
to pre-titrate the solvent and the titration
vessel moisture. Allow the background drift rate to
stabilize before proceeding to the next step.
ANALYSIS
• Fill the syringe and needle with the water standard.
• Weigh the syringe, needle and water standard.
• Press
. You will be prompted to enter the
sample size.
• Dispense 2.00 g (about 2 mL) of standard into the
titration vessel through the septum using the needle.
• Pay attention not to get any sample on the electrode
or beaker wall. If necessary, swirl the titration vessel
gently by hand to remove any standard on the
electrode or beaker wall.
• Clear the needle of residual standard by intaking a
small volume of air from the titration vessel. If a
“hanging drop” of standard is seen on the end of
the needle, dip the end of the needle briefly in the
solvent.
• Remove the needle from the titration vessel and
weigh the syringe again in order to determine the
exact amount of standard added (by difference of
the two measurements.)
• Use the numeric keypad to enter the exact weight
and press
to start the analysis.
• At the end of the titration, the Standardization
Result screen is displayed. The results are expressed
in mg/mL.
CALCULATIONS
Name:
2mg/mL Stdz w/water std
Method Revision:
1.1
Type:
Titrant Standardization
Predispensing Amount:
25 %
Pre-Analysis Stir Time:
5 Sec
Stirring Speed:
900 RPM
Stirbar Type:
Medium
Drift Entry:
Automatic
Solvent:
Methanol
Standard:
Liquid 1.0 mg/g
Type:
Liquid by mass
Concentration Unit:
mg/g
Water Content:
1.0000 mg/g
Standard Size:
2.0000 g
Titrant:
Composite 2
Titrant Type:
one-component
Nominal Titrant Conc.: 2.0000 mg/mL
Std. Titrant Conc.:
2.0000 mg/mL
Date/Time:
Apr 02, 2019 11:45
Titrant Age Reminder:
2d:00h:00m
Control Parameters:
Start Mode:
Normal
Standby Mode:
Enabled
Standby Duration:
12:00 [hh:mm]
Imposed Current:
20 μA
Minimum Dose:
1.000 μL
Maximum Dose:
20.000 μL
Max Dosing Mode
Disabled
Timed Increment:
1 second
End Point Value:
180.0 mV
Signal Averaging:
3 Readings
Flow Rate:
10.0 mL/min
Termination Parameters:
Maximum Duration:
1200 sec
Maximum Titrant Volume: 10.000 mL
Term. Criterion:
Relative Drift
Relative Drift:
7.0 μg/min
Significant Figures
XXXXX
Titrant units:
mg/mL
Titrant volume consumed:
V (mL)
Final Results Units:
mg/mL
Standard Concentration: 1.0000 mg/g
Standard mass:
2.0000 g
RESULTS
3
APPLICATIONS
METHOD PARAMETERS
Method Name: 2mg/mL Stdz w/water std
Time & Date:
Apr 03, 2019 12:00
Standard Size:
2.0000 g
Standard Conc.:
1.0000 mg/g
Drift Value:
5.0 μg/min
End Point Volume:
1.0496 mL
Result:
1.9103 mg/mL
Titration Duration:
5:10 [mm:ss]
Estimated Cell Volume:
60.11 mL
Titration went to Completion
Operator Name:
Analyst Signature:____________________
HI8002EN
3-5
3
HI8003EN 1.0 mg/mL TITRANT STANDARDIZATION WITH WATER STANDARD
HI8003EN
APPLICATIONS
One-Component Titrant
3-6
DESCRIPTION
Method for the standardization (titer determination) of 1.0
mg/mL one-component Karl Fischer titrant using a Liquid
Water Standard. The results are expressed in mg/mL.
ELECTRODE
• HI76320 Dual Platinum Pin Electrode
REAGENTS
• 1 mg/mL one-component Karl Fischer volumetric
titrant
• 1 mg/g Liquid Water Standard
• Dry methanol
ACCESSORIES
• 3 mL syringe (clean and dry)
• 22-gauge, 6” non-coring septum penetration needle
(clean and dry)
• Solvent bottle, GL45 thread
DEVICE PREPARATION
• Connect the solvent bottle top assembly to the bottle
of methanol according to the manual.
• Assemble the titration vessel according to the
instruction manual.
• Install a 5 mL burette filled with 1 mg/mL Karl
Fischer volumetric titrant to be standardized and
verify that no air bubbles are present in the burette
or tubing. If necessary, prime until all air has been
removed completely.
• Press
from the main screen. Use the arrow
keys to highlight HI8003EN 1mg/mL Stdz w/water
std and press
.
• Dispense enough methanol from the solvent bottle
to fill the vessel to the “min” line (about 50 mL).
• Press
to pre-titrate the solvent and the titration
vessel moisture. Allow the background drift rate to
stabilize before proceeding to the next step.
ANALYSIS
• Fill the syringe and needle with the water standard.
• Weigh the syringe, needle and water standard.
• Press
. You will be prompted to enter the
sample size.
• Dispense 2.00 g (about 2 mL) of standard into the
titration vessel through the septum using the needle.
• Pay attention not to get any sample on the electrode
or beaker wall. If necessary, swirl the titration vessel
gently by hand to remove any standard on the
electrode or beaker wall.
• Clear the needle of residual standard by intaking a
small volume of air from the titration vessel. If a
“hanging drop” of standard is seen on the end of
the needle, dip the end of the needle briefly in the
solvent.
• Remove the needle from the titration vessel and
weigh the syringe again in order to determine the
exact amount of standard added (by difference of
the two measurements.)
• Use the numeric keypad to enter the exact weight
and press
to start the analysis.
• At the end of the titration, the Standardization
Result screen is displayed. The results are expressed
in mg/mL.
CALCULATIONS
Name:
1mg/mL Stdz w/water std
Method Revision:
1.1
Type:
Titrant Standardization
Predispensing Amount:
25 %
Pre-Analysis Stir Time:
5 Sec
Stirring Speed:
900 RPM
Stirbar Type:
Medium
Drift Entry:
Automatic
Solvent:
Methanol
Standard:
Liquid 1.0 mg/g
Type:
Liquid by mass
Concentration Unit:
mg/g
Water Content:
1.0000 mg/g
Standard Size:
2.0000 g
Titrant:
Composite 1
Titrant Type:
one-component
Nominal Titrant Conc.: 1.0000 mg/mL
Std. Titrant Conc.:
1.0000 mg/mL
Date/Time:
Apr 02, 2019 11:45
Titrant Age Reminder:
2d:00h:00m
Control Parameters:
Start Mode:
Normal
Standby Mode:
Enabled
Standby Duration:
12:00 [hh:mm]
Imposed Current:
20 μA
Minimum Dose:
2.000 μL
Maximum Dose:
40.000 μL
Max Dosing Mode
Disabled
Timed Increment:
1 second
End Point Value:
180.0 mV
Signal Averaging:
3 Readings
Flow Rate:
10.0 mL/min
Termination Parameters:
Maximum Duration:
1200 sec
Maximum Titrant Volume: 10.000 mL
Term. Criterion:
Relative Drift
Relative Drift:
7.0 μg/min
Significant Figures
XXXXX
Titrant units:
mg/mL
Titrant volume consumed:
V (mL)
Final Results Units:
mg/mL
Standard Concentration: 1.0000 mg/g
Standard mass:
2.0000 g
RESULTS
3
APPLICATIONS
METHOD PARAMETERS
Method Name: 1mg/mL Stdz w/water std
Time & Date:
Apr 03, 2019 12:00
Standard Size:
2.0000 g
Standard Conc.:
1.0000 mg/g
Drift Value:
5.0 μg/min
End Point Volume:
1.8528 mL
Result:
1.0824 mg/mL
Titration Duration:
5:30 [mm:ss]
Estimated Cell Volume:
64.20 mL
Titration went to Completion
Operator Name:
Analyst Signature:____________________
HI8003EN
3-7
3
HI8011EN 5.0 mg/mL TITRANT STANDARDIZATION WITH DISODIUM TARTRATE
HI8011EN
APPLICATIONS
One-Component Titrant
3-8
DESCRIPTION
Method for the standardization (titer determination) of
5.0 mg/mL one-component Karl Fischer titrant using
Disodium Tartrate Dihydrate water standard. The results
are expressed in mg/mL.
ELECTRODE
• HI76320 Dual Platinum Pin Electrode
REAGENTS
• 5 mg/mL one-component Karl Fischer volumetric
titrant
• Disodium Tartrate Dihydrate, 15.66% H2O (w/w)
• Dry methanol
• Dry formamide
ACCESSORIES
• Weigh boat (clean and dry)
• Solvent bottle, GL45 thread
SOLVENT PREPARATION
• Prepare at least 200 mL of solvent. Add dry methanol
and dry formamide 2:1 to the solvent bottle.
DEVICE PREPARATION
• Connect the solvent bottle top assembly to the bottle
of solvent according to the manual.
• Assemble the titration vessel according to the
instruction manual.
• Install a 5 mL burette filled with 5 mg/mL onecomponent Karl Fischer Titrant to be standardized
and verify that no air bubbles are present in the
burette or tubing. If necessary, prime until all air has
been removed completely.
• Press
from the main screen. Use the arrow
keys to highlight HI8011EN 5mg/mL Stdz w/
tartrate and press
.
• Dispense enough solvent from the solvent bottle to
fill the vessel to the “min” line (about 50 mL).
• Press
to pre-titrate the solvent and the titration
vessel moisture. Allow the background drift rate to
stabilize before proceeding to the next step.
ANALYSIS
• Add 0.050 g to 0.100 g of tartrate standard to a
weigh boat.
• Weigh the weigh boat and tartrate standard.
• Press
. You will be prompted to enter the
sample size.
• Quickly remove the sample port plug from the beaker
assembly, pour the tartrate into the titration vessel,
and replace the sample port plug.
• Pay attention not to get any sample on the electrode
or beaker wall. If necessary, swirl the titration vessel
gently by hand to remove any standard on the
electrode or beaker wall.
• Weigh the weigh boat again in order to determine
the exact amount of standard added (by difference
of the two measurements.)
• Use the numeric keypad to enter the exact weight
and press
to start the analysis.
• At the end of the titration the Standardization Result
screen is displayed. The results are expressed in mg/mL.
CALCULATIONS
Name:
5mg/mL Stdz w/tartrate
Method Revision:
1.1
Type:
Titrant Standardization
Predispensing Amount:
15 %
Pre-Analysis Stir Time:
30 Sec
Stirring Speed:
900 RPM
Stirbar Type:
Medium
Drift Entry:
Automatic
Solvent:
MeOH Form. 2:1
Standard:
Sodium Tartrate
Type:
Solid by mass
Concentration Unit:
%
Water Content:
15.66 %
Standard Size:
0.1000 g
Titrant:
Composite 5
Titrant Type:
one-component
Nominal Titrant Conc.: 5.0000 mg/mL
Std. Titrant Conc.:
5.0000 mg/mL
Date/Time:
Apr 02, 2019 11:45
Titrant Age Reminder:
2d:00h:00m
Control Parameters:
Start Mode:
Normal
Standby Mode:
Enabled
Standby Duration:
12:00 [hh:mm]
Imposed Current:
20 μA
Minimum Dose:
2.000 μL
Maximum Dose:
40.000 μL
Max Dosing Mode
Disabled
Timed Increment:
1 second
End Point Value:
180.0 mV
Signal Averaging:
3 Readings
Flow Rate:
10.0 mL/min
Termination Parameters:
Maximum Duration:
1200 sec
Maximum Titrant Volume: 10.000 mL
Term. Criterion:
Relative Drift
Relative Drift:
7.0 μg/min
Significant Figures
XXXXX
Titrant units:
mg/mL
Titrant volume consumed:
V (mL)
Final Results Units:
mg/mL
Standard Concentration:
15.66 %
Standard mass:
0.1000 g[W/W]
RESULTS
3
APPLICATIONS
METHOD PARAMETERS
Method Name: 5mg/mL Stdz w/tartrate
Time & Date:
Apr 03, 2019 12:00
Standard Size:
0.1000 g
Standard Conc.:
15.66 %
Drift Value:
4.0 μg/min
End Point Volume:
3.1333 mL
Result:
5.0329 mg/mL
Titration Duration:
8:48 [mm:ss]
Estimated Cell Volume:
69.26 mL
Titration went to Completion
Operator Name:
Analyst Signature:____________________
HI8011EN
3-9
HI8101EN
APPLICATIONS
3
3-10
HI8101EN MOISTURE DETERMINATION IN DAIRY CREAM
DESCRIPTION
Method for the determination of moisture in dairy cream.
The results are expressed in % mass and should be
between 70 and 80 %.
ELECTRODE
• HI76320 Dual Platinum Pin Electrode
REAGENTS
• 5 mg/mL one-component Karl Fischer volumetric
titrant
• Dry methanol
• Dry chloroform
• Dry formamide
ACCESSORIES
• 1 mL syringe (clean and dry)
• 22-gauge, 6” non-coring septum penetration needle
(clean and dry)
• Solvent bottle, GL45 thread
SOLVENT PREPARATION
• Prepare at least 200 mL of solvent. Add 2 parts dry
chloroform, 2 parts dry methanol and 1 part dry
formamide to the solvent bottle.
DEVICE PREPARATION
• Connect the solvent bottle top assembly to the bottle
of solvent according to the manual.
• Assemble the titration vessel according to the
instruction manual.
• Install a 5 mL burette filled with 5 mg/mL onecomponent Karl Fischer volumetric titrant and verify
that no air bubbles are present in the burette or
tubing. If necessary, prime until all air has been
removed completely.
• Press
from the main screen. Use the arrow
keys to highlight HI8101EN Moisture in Dairy Cream
and press
.
• For the determination of the exact concentration of
the titrant, follow HI8001EN 5mg/mL Stdz w/water
std or HI8011EN 5mg/mL Stdz w/tartrate.
• Dispense enough solvent from the solvent bottle to
fill the vessel to the “min” line (about 50 mL).
• Press
to pre-titrate the solvent and the titration
vessel moisture. Allow the background drift rate to
stabilize before proceeding to the next step.
ANALYSIS
• Fill the syringe and needle with the sample.
• Weigh the syringe, needle and dairy cream.
• Press
. You will be prompted to enter the
sample size.
• Dispense 0.020 g to 0.025 g of dairy cream into the
titration vessel through the septum using the needle.
• Pay attention not to get any sample on the electrode
or beaker wall. If necessary, swirl the titration
vessel gently by hand to remove any sample on the
electrode or beaker wall.
• Clear the needle of residual sample by intaking a
small volume of air from the titration vessel. If a
“hanging drop” of sample is seen on the end of
the needle, dip the end of the needle briefly in the
solvent.
• Remove the needle from the titration vessel and
weigh the syringe again in order to determine
the added sample mass (by difference of the two
measurements.)
• Use the numeric keypad to enter the exact weight
and press
to start the analysis.
• At the end of the titration the Result screen is
displayed. The results are expressed in % mass.
CALCULATIONS
Name:
Moisture in Dairy Cream
Method Revision:
1.1
Type:
Sample Analysis
Predispensing Amount:
30 %
Pre-Analysis Stir Time:
30 Sec
Stirring Speed:
900 RPM
Stirbar Type:
Medium
Drift Entry:
Automatic
Solvent:
Cream Solvent
Sample Parameters:
Sample Determ.:
Normal
Sample Name:
Dairy Cream
Sample Type:
Mass
Sample Size:
0.0250 g
Titrant:
Composite 5
Titrant Type:
one-component
Nominal Titrant Conc.: 5.0000 mg/mL
Std. Titrant Conc.:
5.0000 mg/mL
Date/Time:
Apr 02, 2019 11:45
Titrant Age Reminder:
2d:00h:00m
Control Parameters:
Start Mode:
Normal
Standby Mode:
Enabled
Standby Duration:
12:00 [hh:mm]
Imposed Current:
20 μA
Minimum Dose:
0.500 μL
Maximum Dose:
30.000 μL
Max Dosing Mode
Disabled
Timed Increment:
1 second
End Point Value:
180.0 mV
Signal Averaging:
3 Readings
Flow Rate:
10.0 mL/min
Termination Parameters:
Maximum Duration:
900 sec
Maximum Titrant Volume: 10.000 mL
Term. Criterion:
Relative Drift
Relative Drift:
15.0 μg/min
Result Unit:
%
Significant Figures
XXXXX
Titrant units:
mg/mL
Titrant volume consumed:
V (mL)
Final results units:
% Mass
Titrant concentration: 5.0000 mg/mL
Sample mass:
0.0250 g
RESULTS
3
APPLICATIONS
METHOD PARAMETERS
Method Name: Moisture in Dairy Cream
Time & Date:
Apr 03, 2019 12:00
Sample Size:
0.0241 g
Std. Titrant Conc.:
5.0000 mg/mL
Drift Value:
4.7 μg/min
End Point Volume:
3.4567 mL
Result:
71.5481 %
Titration Duration:
8:36 [mm:ss]
Estimated Cell Volume:
65.72 mL
Titration went to Completion
Operator Name:
Analyst Signature:____________________
HI8101EN
3-11
HI8102EN
APPLICATIONS
3
3-12
HI8102EN MOISTURE DETERMINATION IN MILK
DESCRIPTION
Method for the determination of moisture in milk. The
results are expressed in % mass and should be between
80 and 95 %.
ELECTRODE
• HI76320 Dual Platinum Pin Electrode
REAGENTS
• 5 mg/mL one-component Karl Fischer volumetric
titrant
• Dry methanol
ACCESSORIES
• 1 mL syringe (clean and dry)
• 22-gauge, 6” non-coring septum penetration needle
(clean and dry)
• Solvent bottle, GL45 thread
DEVICE PREPARATION
• Connect the solvent bottle top assembly to the bottle
of methanol according to the manual.
• Assemble the titration vessel according to the
instruction manual.
• Install a 5 mL burette filled with 5 mg/mL onecomponent Karl Fischer volumetric titrant and verify
that no air bubbles are present in the burette or
tubing. If necessary, prime until all air has been
removed completely.
• Press
from the main screen. Use the arrow
keys to highlight HI8102EN Moisture in Milk and
press
.
• For the determination of the exact concentration
of the titrant, follow HI8001EN 5mg/mL Stdz w/
water std or HI8011EN 5mg/mL Stdz w/tartrate.
• Dispense enough methanol from the solvent bottle
to fill the vessel to the “min” line (about 50 mL).
• Press
to pre-titrate the solvent and the titration
vessel moisture. Allow the background drift rate to
stabilize before proceeding to the next step.
ANALYSIS
• Fill the syringe and needle with the sample.
• Weigh the syringe, needle and milk.
• Press
. You will be prompted to enter the
sample size.
• Dispense 0.015 g to 0.020 g of milk into the
titration vessel through the septum using the needle.
• Pay attention not to get any sample on the electrode
or beaker wall. If necessary, swirl the titration
vessel gently by hand to remove any sample on the
electrode or beaker wall.
• Clear the needle of residual sample by intaking a
small volume of air from the titration vessel. If a
“hanging drop” of sample is seen on the end of
the needle, dip the end of the needle briefly in the
solvent.
• Remove the needle from the titration vessel and
weigh the syringe again in order to determine
the added sample mass (by difference of the two
measurements.)
• Use the numeric keypad to enter the exact weight
and press
to start the analysis.
• At the end of the titration the Result screen is
displayed. The results are expressed in % mass of
water.
CALCULATIONS
Name:
Moisture in Milk
Method Revision:
1.1
Type:
Sample Analysis
Predispensing Amount:
30 %
Pre-Analysis Stir Time:
15 Sec
Stirring Speed:
900 RPM
Stirbar Type:
Medium
Drift Entry:
Automatic
Solvent:
Methanol
Sample Parameters:
Sample Determ.:
Normal
Sample Name:
Milk
Sample Type:
Mass
Sample Size:
0.0200 g
Titrant:
Composite 5
Titrant Type:
one-component
Nominal Titrant Conc.: 5.0000 mg/mL
Std. Titrant Conc.:
5.0000 mg/mL
Date/Time:
Apr 02, 2019 11:45
Titrant Age Reminder:
2d:00h:00m
Control Parameters:
Start Mode:
Normal
Standby Mode:
Enabled
Standby Duration:12:00 [hh:mm]
Imposed Current:
20 μA
Minimum Dose:
0.500 μL
Maximum Dose:
40.000 μL
Max Dosing Mode
Disabled
Timed Increment:
1 second
End Point Value:
180.0 mV
Signal Averaging:
3 Readings
Flow Rate:
10.0 mL/min
Termination Parameters:
Maximum Duration:
900 sec
Maximum Titrant Volume: 10.000 mL
Term. Criterion:
Relative Drift
Relative Drift:
15.0 μg/min
Result Unit:
%
Significant Figures
XXXXX
Titrant units:
mg/mL
Titrant volume consumed:
V (mL)
Final results units:
% Mass
Titrant concentration: 5.0000 mg/mL
Sample mass:
0.0200 g
RESULTS
3
APPLICATIONS
METHOD PARAMETERS
Method Name:
Moisture in Milk
Time & Date:
Apr 03, 2019 12:00
Sample Size:
0.0188 g
Std. Titrant Conc.:
5.0000 mg/mL
Drift Value:
4.5 μg/min
End Point Volume:
3.2614 mL
Result:
86.5886 %
Titration Duration:
6:18 [mm:ss]
Estimated Cell Volume:
60.03 mL
Titration went to Completion
Operator Name:
Analyst Signature:____________________
HI8102EN
3-13
HI8103EN
APPLICATIONS
3
3-14
HI8103EN MOISTURE DETERMINATION IN HONEY
DESCRIPTION
Method for the determination of moisture in honey. The
results are expressed in % mass and should be between
15 and 20 %.
ELECTRODE
• HI76320 Dual Platinum Pin Electrode
REAGENTS
• 5 mg/mL one-component Karl Fischer volumetric
titrant
• Dry methanol
ACCESSORIES
• 1 mL syringe (clean and dry)
• Solvent bottle, GL45 thread
DEVICE PREPARATION
• Connect the solvent bottle top assembly to the bottle
of methanol according to the manual.
• Assemble the titration vessel according to the
instruction manual.
• Install a 5 mL burette filled with 5 mg/mL onecomponent Karl Fischer volumetric titrant and verify
that no air bubbles are present in the burette or
tubing. If necessary, prime until all air has been
removed completely.
• Press
from the main screen. Use the arrow
keys to highlight HI8103EN Moisture in Honey and
press
.
• For the determination of the exact concentration
of the titrant, follow HI8001EN 5mg/mL Stdz w/
water std or HI8011EN 5mg/mL Stdz w/tartrate.
• Dispense enough methanol from the solvent bottle
to fill the vessel to the “min” line (about 50 mL).
• Press
to pre-titrate the solvent and the titration
vessel moisture. Allow the background drift rate to
stabilize before proceeding to the next step.
ANALYSIS
• Fill the syringe with the sample.
• Weigh the syringe, needle and honey.
• Press
. You will be prompted to enter the
sample size.
• Remove the sample port plug and dispense 0.050 g
to 0.100 g of honey (about 2-3 small drops) into the
titration vessel through the sample port. Replace the
sample port plug as quickly as possible to prevent
humidity from entering the titration beaker.
• Pay attention not to get any sample on the electrode
or beaker wall. If necessary, swirl the titration
vessel gently by hand to remove any sample on the
electrode or beaker wall.
• Weigh the syringe again in order to determine
the added sample mass (by difference of the two
measurements.)
• Use the numeric keypad to enter the exact weight
and press
to start the analysis.
• At the end of the titration the Result screen is
displayed. The results are expressed in % mass of
water.
Name:
Moisture in Honey
Method Revision:
1.1
Type:
Sample Analysis
Predispensing Amount:
None
Pre-Analysis Stir Time:
60 Sec
Stirring Speed:
900 RPM
Stirbar Type:
Medium
Drift Entry:
Automatic
Solvent:
Methanol
Sample Parameters:
Sample Determ.:
Normal
Sample Name:
Honey
Sample Type:
Mass
Sample Size:
0.1000 g
Titrant:
Composite 5
Titrant Type:
one-component
Nominal Titrant Conc.: 5.0000 mg/mL
Std. Titrant Conc.:
5.0000 mg/mL
Date/Time:
Apr 02, 2019 11:45
Titrant Age Reminder:
2d:00h:00m
Control Parameters:
Start Mode:
Normal
Standby Mode:
Enabled
Standby Duration:
12:00 [hh:mm]
Imposed Current:
20 μA
Minimum Dose:
0.500 μL
Maximum Dose:
20.000 μL
Max Dosing Mode
Disabled
Timed Increment:
1 second
End Point Value:
180.0 mV
Signal Averaging:
3 Readings
Flow Rate:
10.0 mL/min
Termination Parameters:
Maximum Duration:
900 sec
Maximum Titrant Volume: 10.000 mL
Term. Criterion:
Relative Drift
Relative Drift:
10.0 μg/min
Result Unit:
%
Significant Figures
XXXXX
Titrant units:
mg/mL
Titrant volume consumed:
V (mL)
Final results units:
% Mass
Titrant concentration: 5.0000 mg/mL
Sample mass:
0.1000 g
RESULTS
Method Name:
Moisture in Honey
Time & Date:
Apr 03, 2019 12:00
Sample Size:
0.0916 g
Std. Titrant Conc.:
5.0000 mg/mL
Drift Value:
3.8 μg/min
End Point Volume:
3.4523 mL
Result:
17.2345 %
Titration Duration:
7:06 [mm:ss]
Estimated Cell Volume:
57.16 mL
Titration went to Completion
Operator Name:
Analyst Signature:____________________
3
HI8103EN
CALCULATIONS
APPLICATIONS
METHOD PARAMETERS
3-15
HI8104EN
APPLICATIONS
3
3-16
HI8104EN SURFACE MOISTURE DETERMINATION ON WHITE SUGAR
DESCRIPTION
Method for the determination of the surface moisture
content of white sugar. The results are expressed in ppm
and should be between 250 and 350 ppm.
ELECTRODE
• HI76320 Dual Platinum Pin Electrode
REAGENTS
• 1 mg/mL one-component Karl Fischer volumetric
titrant
• Dry methanol
• Dry chloroform
ACCESSORIES
• Weigh boat (clean and dry)
• Solvent bottle, GL45 thread
SOLVENT PREPARATION
• Prepare at least 200 mL of solvent. Add 2 parts dry
chloroform and 1 part dry methanol to the solvent
bottle.
DEVICE PREPARATION
• Connect the solvent bottle top assembly to the bottle
of solvent according to the manual.
• Assemble the titration vessel according to the
instruction manual.
• Install a 5 mL burette filled with 1 mg/mL onecomponent Karl Fischer volumetric titrant and verify
that no air bubbles are present in the burette or
tubing. If necessary, prime until all air has been
removed completely.
• Press
from the main screen. Use the arrow
keys to highlight HI8104EN Surface Moisture Sugar and press
.
• For the determination of the exact concentration of
the titrant follow HI8003EN 1mg/mL Stdz w/water
std.
• Dispense enough solvent from the solvent bottle to
fill the vessel to the “min” line (about 50 mL).
• Press
to pre-titrate the solvent and the titration
vessel moisture. Allow the background drift rate to
stabilize before proceeding to the next step.
ANALYSIS
• Fill the weigh boat with 7.5 to 10.0 g of sample.
• Weigh the weigh boat and sample.
• Press
. You will be prompted to enter the
sample size.
• Remove the sample port and use the weight boat
to transfer the solid sample into the titration vessel.
Replace the sample port plug as quickly as possible
to prevent humidity from entering the titration
beaker.
• Pay attention not to get any sample on the electrode
or beaker wall. If necessary, swirl the titration
vessel gently by hand to remove any sample on the
electrode or beaker wall.
• Weigh the weigh boat again in order to determine
the added sample mass (by difference of the two
measurements.)
• Use the numeric keypad to enter the exact weight
and press
to start the analysis.
• At the end of the titration the Result screen is
displayed. The results are expressed in ppm of water.
• Replace the solvent after 2 to 3 titrations.
CALCULATIONS
Name:
Surface Moisture - Sugar
Method Revision:
1.1
Type:
Sample Analysis
Predispensing Amount:
None
Pre-Analysis Stir Time:
120 Sec
Stirring Speed:
900 RPM
Stirbar Type:
Medium
Drift Entry:
Automatic
Solvent:
CHCl3 MeOH 2:1
Sample Parameters:
Sample Determ.:
Normal
Sample Name:
Sugar
Sample Type:
Mass
Sample Size:
7.5000 g
Titrant:
Composite 1
Titrant Type: one-component
Nominal Titrant Conc.: 1.0000 mg/mL
Std. Titrant Conc.:
1.0000 mg/mL
Date/Time:
Apr 02, 2019 11:45
Titrant Age Reminder:
2d:00h:00m
Control Parameters:
Start Mode:
Normal
Standby Mode:
Enabled
Standby Duration:
12:00 [hh:mm]
Imposed Current:
20 μA
Minimum Dose:
1.000 μL
Maximum Dose:
30.000 μL
Max Dosing Mode
Disabled
Timed Increment:
1 second
End Point Value:
180.0 mV
Signal Averaging:
3 Readings
Flow Rate:
10.0 mL/min
Termination Parameters:
Maximum Duration:
900 sec
Maximum Titrant Volume: 10.000 mL
Term. Criterion:
Relative Drift
Relative Drift:
20.0 μg/min
Result Unit:
ppm
Significant Figures
XXXXX
Calculations:
Titrant units:
mg/mL
Titrant volume consumed:
V (mL)
Final results units:
ppm
Titrant concentration: 1.0000 mg/mL
Sample mass:
7.5000 g
ppm =
V × 1.0000 × 1000
7.500
RESULTS
3
APPLICATIONS
METHOD PARAMETERS
Method Name: Surface Moisture-Sugar
Time & Date:
Apr 03, 2019 12:00
Sample Size:
7.5231 g
Std. Titrant Conc.:
1.0000 mg/mL
Drift Value:
5.7 μg/min
End Point Volume:
2.4292 mL
Result:
319 ppm
Titration Duration:
4:42 [mm:ss]
Estimated Cell Volume:
62.4 mL
Titration went to Completion
Operator Name:
Analyst Signature:____________________
HI8104EN
3-17
HI8105EN
APPLICATIONS
3
3-18
HI8105EN MOISTURE DETERMINATION IN COOKING OIL
DESCRIPTION
Method for the determination of moisture in cooking oil.
The results are expressed in ppm and should be between
200 and 800 ppm.
ELECTRODE
• HI76320 Dual Platinum Pin Electrode
REAGENTS
• 1 mg/mL one-component Karl Fischer volumetric
titrant
• Dry methanol
• Dry chloroform
ACCESSORIES
• 25 mL syringe (clean and dry)
• 18-gauge, 6” non-coring septum penetration needle
(clean and dry)
• Solvent bottle, GL45 thread
SOLVENT PREPARATION
• Prepare at least 200 mL of solvent. Add equal parts
of dry chloroform and dry methanol to the solvent
bottle.
DEVICE PREPARATION
• Connect the solvent bottle top assembly to the bottle
of solvent according to the manual.
• Assemble the titration vessel according to the
instruction manual.
• Install a 5 mL burette filled with 1 mg/mL onecomponent Karl Fischer volumetric titrant and verify
that no air bubbles are present in the burette or
tubing. If necessary, prime until all air has been
removed completely.
• Press
from the main screen. Use the arrow
keys to highlight HI8105EN Moisture in Cooking Oil
and press
.
• For the determination of the exact concentration of
the titrant follow HI8003EN 1mg/mL Stdz w/water
std.
• Dispense enough solvent from the solvent bottle to
fill the vessel to the “min” line (about 50 mL).
• Press
to pre-titrate the solvent and the titration
vessel moisture. Allow the background drift rate to
stabilize before proceeding to the next step.
ANALYSIS
• Fill the syringe and needle with sample.
• Weigh the syringe, needle and oil.
• Press
. You will be prompted to enter the
sample size.
• Dispense 3.0 g to 5.0 g of cooking oil into the
titration vessel through the septum using the needle.
• Pay attention not to get any sample on the electrode
or beaker wall. If necessary, swirl the titration
vessel gently by hand to remove any sample on the
electrode or beaker wall.
• Clear the needle of residual sample by intaking a
small volume of air from the titration vessel. If a
“hanging drop” of sample is seen on the end of
the needle, dip the end of the needle briefly in the
solvent.
• Remove the needle from the titration vessel and
weigh the syringe again in order to determine
the added sample mass (by difference of the two
measurements.)
• Use the numeric keypad to enter the exact weight
and press
to start the analysis.
• At the end of the titration the Result screen is
displayed. The results are expressed in ppm of water.
• Replace the solvent after 3 to 4 titrations, or if
phase-separation occurs.
CALCULATIONS
Name:
Moisture in Cooking Oil
Method Revision:
1.1
Type:
Sample Analysis
Predispensing Amount:
None
Pre-Analysis Stir Time:
15 Sec
Stirring Speed:
900 RPM
Stirbar Type:
Medium
Drift Entry:
Automatic
Solvent:
CHCl3 MeOH 1:1
Sample Parameters:
Sample Determ.:
Normal
Sample Name:
Oil
Sample Type:
Mass
Sample Size:
4.0000 g
Titrant:
Composite 1
Titrant Type:
one-component
Nominal Titrant Conc.: 1.0000 mg/mL
Std. Titrant Conc.:
1.0000 mg/mL
Date/Time:
Apr 02, 2019 11:45
Titrant Age Reminder:
2d:00h:00m
Control Parameters:
Start Mode:
Cautious
Standby Mode:
Enabled
Standby Duration:
12:00 [hh:mm]
Imposed Current:
20 μA
Minimum Dose:
1.000 μL
Maximum Dose:
30.000 μL
Max Dosing Mode
Disabled
Timed Increment:
1 second
End Point Value:
180.0 mV
Signal Averaging:
3 Readings
Flow Rate:
10.0 mL/min
Termination Parameters:
Maximum Duration:
900 sec
Maximum Titrant Volume: 10.000 mL
Term. Criterion:
Relative Drift
Relative Drift:
10.0 μg/min
Result Unit:
ppm
Significant Figures
XXXXX
Calculations:
Titrant units:
mg/mL
Titrant volume consumed:
V (mL)
Final results units:
ppm
Titrant concentration: 1.0000 mg/mL
Sample mass:
4.0000 g
RESULTS
3
APPLICATIONS
METHOD PARAMETERS
Method Name: Moisture in Cooking Oil
Time & Date:
Apr 03, 2019 12:00
Sample Size:
4.0296 g
Std. Titrant Conc.:
1.0000 mg/mL
Drift Value:
3.4 μg/min
End Point Volume:
2.6808 mL
Result:
664 ppm
Titration Duration:
6:30 [mm:ss]
Estimated Cell Volume:
58.11 mL
Titration went to Completion
Operator Name:
Analyst Signature:____________________
HI8105EN
3-19
3
HI8106EN MOISTURE DETERMINATION IN BUTTER
HI8106EN
APPLICATIONS
By External Dissolution
3-20
DESCRIPTION
Method for the determination of moisture in butter by
external dissolution. The results are expressed in % mass
and should be between 15 and 20 %.
ELECTRODE
• HI76320 Dual Platinum Pin Electrode
REAGENTS
• 5 mg/mL one-component Karl Fischer volumetric
titrant
• Dry methanol
• Dry chloroform
ACCESSORIES
• 1 mL syringe (clean and dry)
• 22-gauge, 6” non-coring septum penetration needle
(clean and dry)
• Solvent bottle, GL45 thread
• 100 mL dissolution bottle with septum
• Magnetic stirrer and stirbar
EXTERNAL DISSOLUTION PROCEDURE
• To an external dissolution bottle with septum, add a
magnetic stir bar. Weigh the bottle and record this
value.
• Add 15 g of dry methanol and 25 g of dry chloroform
to the bottle and stir for 15 to 20 minutes.
• Follow HI8301EN Solvent w/ 5 mg/mL 1-comp. to
determine the moisture content of the solvent mixture.
• Enter the solvent moisture concentration by pressing
,then Sample Parameters, External Solvent
Concentration. Use the numeric keypad to enter the
exact concentration. Press
or
.
• Weigh the dissolution bottle to determine the weight of
the remaining solvent (by subtracting the empty bottle
mass). Enter the exact mass in Sample Parameters,
External Solvent Size. Use the numeric keypad to enter
the exact mass. Press
or
.
• Add 2.0 to 4.0 g of butter to the bottle. Weigh the
bottle to determine the exact dissoluted sample
weight. Enter the exact mass in Sample Parameters,
Dissoluted Sample Size. Use the numeric keypad to
enter the exact mass. Press
or
.
• Replace the cap and mix for 20 to 30 minutes, to
dissolve the sample. The resulting solution will be
used to determine the water content.
Note: Titrate the solution immediately.
DEVICE PREPARATION
• Connect the solvent bottle top assembly to the bottle
of methanol according to the manual.
• Assemble the titration vessel according to the
instruction manual.
• Press
from the main screen. Use the arrow
keys to highlight HI8106EN Moisture in Butter and
press
.
• Install a 5 mL burette filled with 5 mg/mL onecomponent Karl Fischer volumetric titrant and verify
that no air bubbles are present in the burette or
tubing. If necessary, prime until all air has been
removed completely.
• To determine the exact concentration of the titrant
follow HI8001EN 5mg/mL Stdz w/water std or
HI8011EN 5mg/mL Stdz w/tartrate.
• Dispense enough methanol from the solvent bottle
to fill the vessel to the “min” line (about 50 mL).
• Press
to pre-titrate the titration solvent and the
titration vessel moisture. Allow the background drift
rate to stabilize before proceeding to the next step.
• Stop stirring the dissolution bottle and allow any
particulate matter to settle.
ANALYSIS
• Fill the syringe and needle with supernatant through
the septum on the dissolution bottle.
• Weigh the syringe, needle and supernatant.
• Press
. You will be prompted to enter the
sample size.
• Dispense 0.500 g to 1.000 g of sample solution
into the titration vessel through the septum using
the needle.
the added sample mass (by difference of the two
measurements.)
• Use the numeric keypad to enter the exact weight
and press
to start the analysis.
• At the end of the titration the Result screen is displayed.
The results are expressed in % mass of water.
• Replace the solvent after 10 to 12 titrations.
METHOD PARAMETERS
CALCULATIONS
Name:
Moisture in Butter
Method Revision:
1.1
Type:
Sample Analysis
Predispensing Amount:
None
Pre-Analysis Stir Time:
10 Sec
Stirring Speed:
900 RPM
Stirbar Type:
Medium
Drift Entry:
Automatic
Solvent:
Methanol
Sample Parameters:
Sample Determ.:External Dissolution
Sample Name:
Butter
Sample Size:
0.7500 g
External Solvent Size:
40.0000 g
External Solvent Conc.:
0.0100 %
Extracted Sample Size:
3.0000 g
Titrant:
Composite 5
Titrant Type:
one-component
Nominal Titrant Conc.: 5.0000 mg/mL
Std. Titrant Conc.:
5.0000 mg/mL
Date/Time:
Apr 02, 2019 11:45
Titrant Age Reminder:
2d:00h:00m
Control Parameters:
Start Mode:
Normal
Standby Mode:
Enabled
Standby Duration:
12:00 [hh:mm]
Imposed Current:
20 μA
Minimum Dose:
0.500 μL
Maximum Dose:
40.000 μL
Max Dosing Mode
Disabled
Timed Increment:
1 second
End Point Value:
180.0 mV
Signal Averaging:
3 Readings
Flow Rate:
10.0 mL/min
Termination Parameters:
Maximum Duration:
720 sec
Maximum Titrant Volume: 10.000 mL
Term. Criterion:
Relative Drift
Relative Drift:
15.0 μg/min
Result Unit:
%
Significant Figures
XXXXX
Titrant units:
mg/mL
Titrant volume consumed:
V (mL)
Final results units:
% Mass
Titrant concentration: 5.0000 mg/mL
External Solvent Size:
40.0000 g
External Solvent Conc.:
0.0100 %
Extracted Sample Size:
3.0000 g
Sample mass:
0.7500 g
%% Mass =
3
APPLICATIONS
• Pay attention not to get any sample on the electrode
or beaker wall. If necessary, swirl the titration
vessel gently by hand to remove any sample on the
electrode or beaker wall.
• Clear the needle of residual sample by intaking a small
volume of air from the titration vessel. If a “hanging
drop” of sample is seen on the end of the needle, dip
the end of the needle briefly in the solvent.
• Remove the needle from the titration vessel and
weigh the syringe again in order to determine
5.0000 × V
40.000 �0.7500 × 10� - 0.0100
×
× 100
5.0000 × V
3.000
100 - �
�
0.7500 × 10
RESULTS
HI8106EN
VMoisture
× 5.0000
Method Name:
in Butter
% Mass =
1.0000
× 10 2019 12:00
Time & Date:
Apr 03,
Sample Size:
0.7841 g
Std. Titrant Conc.:
5.0000 mg/mL
Drift Value:
4.6 μg/min
End Point Volume:
2.4497 mL
External Solvent Size:
38.4979 g
External Solvent Conc.:
0.0167 %
Extracted Sample Size:
3.1222 g
Result:
19.3903 %
Titration Duration:
6:54 [mm:ss]
Estimated Cell Volume:
61.0 mL
Titration went to Completion
Operator Name:
Analyst Signature:____________________
3-21
3
HI8107EN MOISTURE DETERMINATION IN MARGARINE
HI8107EN
APPLICATIONS
By External Dissolution
3-22
DESCRIPTION
Method for the determination of moisture in margarine
by external dissolution. The results are expressed in %
mass and should be between 15 and 30 %.
ELECTRODE
• HI76320 Dual Platinum Pin Electrode
REAGENTS
• 5 mg/mL one-component Karl Fischer volumetric
titrant
• Dry methanol
• Dry chloroform
ACCESSORIES
• 1 mL syringe (clean and dry)
• 22-gauge, 6” non-coring septum penetration needle
(clean and dry)
• Solvent bottle, GL45 thread
• 100 mL dissolution bottle with septum
• Magnetic stirrer and stirbar
EXTERNAL DISSOLUTION PROCEDURE
• To an external dissolution bottle with septum, add a
magnetic stir bar. Weigh the bottle and record this
value.
• Add 20 g of dry methanol and 20 g of dry chloroform
to the bottle and stir for 15 to 20 minutes.
• Follow HI8301EN Solvent w/ 5 mg/mL 1-comp.
to determine the moisture content of the solvent
mixture.
• Enter the solvent moisture concentration by pressing
,then Sample Parameters, External Solvent
Concentration. Use the numeric keypad to enter the
exact concentration. Press
or
.
• Weigh the dissolution bottle to determine the
weight of the remaining solvent (by subtracting the
empty bottle mass). Enter the exact mass in Sample
Parameters, External Solvent Size. Use the numeric
keypad to enter the exact mass. Press
or
.
• Add 2.0 to 4.0 g of margarine to the bottle. Weigh
the bottle to determine the exact dissoluted sample
weight. Enter the exact mass in Sample Parameters,
Dissoluted Sample Size. Use the numeric keypad to
enter the exact mass. Press
or
.
• Replace the cap and mix for 20 to 30 minutes to
dissolve the sample. The resulting solution will be
used to determine the water content.
Note: Titrate the solution immediately.
DEVICE PREPARATION
• Connect the solvent bottle top assembly to the bottle
of methanol according to the manual.
• Assemble the titration vessel according to the
instruction manual.
• Press
from the main screen. Use the arrow
keys to highlight HI8107EN Moisture in Margarine
and press
.
• Install a 5 mL burette filled with 5 mg/mL onecomponent Karl Fischer volumetric titrant and verify
that no air bubbles are present in the burette or
tubing. If necessary, prime until all air has been
removed completely.
• For the determination of the exact concentration of
the titrant, follow HI8001EN 5mg/mL Stdz w/water
std or HI8011EN 5mg/mL Stdz w/tartrate.
• Dispense enough methanol from the solvent bottle
to fill the vessel to the “min” line (about 50 mL).
• Press
to pre-titrate the titration solvent and the
titration vessel moisture. Allow the background drift
rate to stabilize before proceeding to the next step.
• Stop stirring the extraction bottle and allow any
particulate matter to settle.
ANALYSIS
• Fill the syringe and needle with the supernatant
through the septum on the dissolution bottle.
• Weigh the syringe, needle and supernatant.
• Press
. You will be prompted to enter the
sample size.
• Dispense 0.500 g to 1.000 g of supernatant into the
titration vessel through the septum using the needle.
• Remove the needle from the titration
vessel and weigh the syringe again in
order to determine the added sample mass
(by difference of the two measurements.)
• Use the numeric keypad to enter the exact weight
and press
to start the analysis.
• At the end of the titration the Result screen is displayed.
The results are expressed in % mass of water.
• Replace the solvent after 12 to 16 titrations.
METHOD PARAMETERS
CALCULATIONS
HI8107EN
Name:
Moisture in Margarine
Titrant units:
mg/mL
Method Revision:
1.1
Titrant volume consumed:
V (mL)
Type:
Sample Analysis
Final results units:
% Mass
Predispensing Amount:
None
Titrant concentration: 5.0000 mg/mL
Pre-Analysis Stir Time:
10 Sec
External Solvent Size:
40.0000 g
Stirring Speed:
900 RPM
External Solvent Conc.:
0.0100 %
Stirbar Type:
Medium
Extracted Sample Size:
3.0000 g
Drift Entry:
Automatic
Sample mass:
0.7500 g
Solvent:
Methanol
5.0000 × V
5.0000 × V
40.000 �0.7500 × 10� - 0.0100
Sample Parameters:
40.000 �0.7500 × 10� -%0.0100
Mass =
×
× 100
%
5.0000 × V
3.000
% Mass
=
×
× 100
Sample Determ.:
External
Extraction
100 - �
�
5.0000 × V
3.000
0.7500
×
10
100 - �
�
Sample Name:
Margarine
0.7500 × 10
Sample Size:
0.7500 g
RESULTS
External Solvent Size:
40.0000 g
V × 5.0000in Margarine
Method Name:
Moisture
External Solvent Conc.:
0.0100
%
V × 5.0000
% Mass =
1.0000
10 2019 12:00
% Mass =
Time
&
Date:
Apr ×03,
Extracted Sample Size:
3.0000
g × 10
1.0000
Sample
Size:
0.7402 g
Titrant:
Composite 5
Std.
Titrant
Conc.:
5.0000
mg/mL
Titrant Type:
one-component
Drift
Value:
4.1
μg/min
Nominal Titrant Conc.: 5.0000 mg/mL
End Point Volume:
3.1402 mL
Std. Titrant Conc.:
5.0000 mg/mL
External
Solvent
Size:
39.9262 g
Date/Time:
Apr 02, 2019 11:45
External
Solvent
Conc.:
0.0141 %
Titrant Age Reminder:
2d:00h:00m
Extracted
Sample
Size:
3.1118 g
Control Parameters:
Result:
27.6339
%
Start Mode:
Normal
Titration
Duration:
5:30
[mm:ss]
Standby Mode:
Enabled
Estimated Cell Volume:
64.4 mL
Standby Duration:
12:00 [hh:mm]
Titration
went
to
Completion
Imposed Current:
20 μA
Operator Name:
Minimum Dose:
1.00 μL
Analyst Signature:____________________
Maximum Dose:
50.000 μL
Max Dosing Mode
Disabled
Timed Increment:
1 second
End Point Value:
180.0 mV
Signal Averaging:
3 Readings
Flow Rate:
10.0 mL/min
Termination Parameters:
Maximum Duration:
720 sec
Maximum Titrant Volume: 10.000 mL
Term. Criterion:
Relative Drift
Relative Drift:
15.0 μg/min
Result Unit:
%
Significant Figures
XXXXX
3
APPLICATIONS
• Pay attention not to get any sample on the electrode
or beaker wall. If necessary, swirl the titration
vessel gently by hand to remove any sample on the
electrode or beaker wall.
• Clear the needle of residual sample by intaking a small
volume of air from the titration vessel. If a “hanging
drop” of sample is seen on the end of the needle, dip
the end of the needle briefly in the solvent.
3-23
HI8108EN
APPLICATIONS
3
3-24
HI8108EN MOISTURE DETERMINATION IN MAYONNAISE
DESCRIPTION
Method for the determination of moisture in Mayonnaise
by external extraction. The results are expressed in %
mass and should be between 40 and 60 %.
ELECTRODE
• HI76320 Dual Platinum Pin Electrode
REAGENTS
• 5 mg/mL one-component Karl Fischer volumetric
titrant
• Dry methanol
ACCESSORIES
• 1 mL syringe (clean and dry)
• 22-gauge, 6” non-coring septum penetration needle
(clean and dry)
• Solvent bottle, GL45 thread
• 100 mL extraction bottle with septum
• Magnetic stirrer and stirbar
EXTERNAL EXTRACTION PROCEDURE
• To an external dissolution bottle with septum, add a
magnetic stir bar. Weigh the bottle and record this
value.
• Add 40 g of dry methanol to the bottle and stir for
5 minutes.
• Follow HI8301EN Solvent w/ 5 mg/mL 1-comp.
to determine the moisture content of the solvent
mixture.
• Enter the solvent moisture concentration by pressing
,then Sample Parameters, External Solvent
Concentration. Use the numeric keypad to enter the
exact concentration. Press
or
.
• Weigh the dissolution bottle to determine the
weight of the remaining solvent (by subtracting the
empty bottle mass). Enter the exact mass in Sample
Parameters, External Solvent Size. Use the numeric
keypad to enter the exact mass. Press
or
.
• Add 0.8 to 1.2 g of mayonnaise to the bottle. Weigh
the bottle to determine the exact dissoluted sample
weight. Enter the exact mass in Sample Parameters,
Dissoluted Sample Size. Use the numeric keypad to
enter the exact mass. Press
or
.
• Replace the cap and mix for 20 to 30 minutes to
dissolve the sample. The resulting solution will be
used to determine the water content.
Note: Titrate the solution immediately.
DEVICE PREPARATION
• Connect the solvent bottle top assembly to the bottle
of methanol according to the manual.
• Assemble the titration vessel according to the
instruction manual.
• Press
from the main screen. Use the arrow
keys to highlight HI8108EN Moisture in Mayonnaise
and press
.
• Install a 5 mL burette filled with 5 mg/mL onecomponent Karl Fischer volumetric titrant and verify
that no air bubbles are present in the burette or
tubing. If necessary, prime until all air has been
removed completely.
• For the determination of the exact concentration
of the titrant, follow HI8001EN 5mg/mL Stdz w/
water std or HI8011EN 5mg/mL Stdz w/tartrate.
• Dispense enough methanol from the solvent bottle
to fill the vessel to the “min” line (about 50 mL).
• Press
to pre-titrate the titration solvent and the
titration vessel moisture. Allow the background drift
rate to stabilize before proceeding to the next step.
• Stop stirring the sample in the extraction bottle and
allow any particulate matter to settle.
ANALYSIS
• Fill the syringe and needle with the supernatant
through the septum on the dissolution bottle.
• Weigh the syringe, needle and supernatant.
• Press
. You will be prompted to enter the
sample size.
• Dispense 0.500 g to 1.000 g of supernatant into the
titration vessel through the septum using the needle.
• Pay attention not to get any sample on the electrode
or beaker wall. If necessary, swirl the titration
the added sample mass (by difference of the two
measurements.)
• Use the numeric keypad to enter the exact weight
and press
to start the analysis.
• At the end of the titration the Result screen is
displayed. The results are expressed in % mass of
water.
• Replace the solvent after 12 to 16 titrations.
METHOD PARAMETERS
CALCULATIONS
Name:
Moisture in Mayonnaise
Method Revision:
1.1
Type:
Sample Analysis
Predispensing Amount:
None
Pre-Analysis Stir Time:
10 Sec
Stirring Speed:
900 RPM
Stirbar Type:
Medium
Drift Entry:
Automatic
Solvent:
Methanol
Sample Parameters:
Sample Determ.: External Extraction
Sample Name:
Mayonnaise
Sample Size:
0.7500 g
External Solvent Size:
40.0000 g
External Solvent Conc.:
0.0100 %
Extracted Sample Size:
1.0000 g
Titrant:
Composite 5
Titrant Type:
one-component
Nominal Titrant Conc.: 5.0000 mg/mL
Std. Titrant Conc.:
5.0000 mg/mL
Date/Time:
Apr 02, 2019 11:45
Titrant Age Reminder:
2d:00h:00m
Control Parameters:
Start Mode:
Normal
Standby Mode:
Enabled
Standby Duration:
12:00 [hh:mm]
Imposed Current:
20 μA
Minimum Dose:
0.500 μL
Maximum Dose:
20.000 μL
Max Dosing Mode
Disabled
Timed Increment:
1 second
End Point Value:
180.0 mV
Signal Averaging:
3 Readings
Flow Rate:
10.0 mL/min
Termination Parameters:
Maximum Duration:
720 sec
Maximum Titrant Volume: 10.000 mL
Term. Criterion:
Relative Drift
Relative Drift:
10.0 μg/min
Result Unit:
%
Significant Figures
XXXXX
Titrant units:
mg/mL
Titrant volume consumed:
V (mL)
Final results units:
% Mass
Titrant concentration: 5.0000 mg/mL
External Solvent Size:
40.0000 g
External Solvent Conc.:
0.0100 %
Extracted Sample Size:
1.0000 g
Sample mass:
0.7500 g
%% Mass =
3
APPLICATIONS
vessel gently by hand to remove any sample on the
electrode or beaker wall.
• Clear the needle of residual sample by intaking a
small volume of air from the titration vessel. If a
“hanging drop” of sample is seen on the end of
the needle, dip the end of the needle briefly in the
solvent.
• Remove the needle from the titration vessel and
weigh the syringe again in order to determine
5.0000 × V
40.000 �0.7500 × 10� - 0.0100
×
× 100
5.0000 × V
3.000
100 - �
�
0.7500 × 10
RESULTS
HI8108EN
V × 5.0000
Method Name:
Moisture
in Mayonnaise
% Mass =
1.0000
× 10 2019 12:00
Time & Date:
Apr 03,
Sample Size:
0.7500 g
Std. Titrant Conc.:
5.0000 mg/mL
Drift Value:
4.6 μg/min
End Point Volume:
2.2010 mL
External Solvent Size:
40.0000 g
External Solvent Conc.:
0.0100 %
Extracted Sample Size:
1.0000 g
Result:
58.9770 %
Titration Duration:
7:18 [mm:ss]
Estimated Cell Volume:
60.0 mL
Titration went to Completion
Operator Name:
Analyst Signature:____________________
3-25
HI8201EN
APPLICATIONS
3
3-26
HI8201EN MOISTURE DETERMINATION IN SHAMPOO
DESCRIPTION
Method for the determination of water in shampoo. The
results are expressed in % mass and should be between
70 and 90 %.
ELECTRODE
• HI76320 Dual Platinum Pin Electrode
REAGENTS
• 5 mg/mL one-component Karl Fischer volumetric
titrant
• Dry methanol
ACCESSORIES
• 1 mL syringe (clean and dry)
• 18-gauge, 6” non-coring septum penetration needle
(clean and dry)
• Solvent bottle, GL45 thread
DEVICE PREPARATION
• Connect the solvent bottle top assembly to the bottle
of methanol according to the manual.
• Assemble the titration vessel according to the
instruction manual.
• Install a 5 mL burette filled with 5 mg/mL onecomponent Karl Fischer volumetric titrant and verify
that no air bubbles are present in the burette or
tubing. If necessary, prime until all air has been
removed completely.
• Press
from the main screen. Use the arrow
keys to highlight HI8201EN Moisture in Shampoo
and press
.
• For the determination of the exact concentration
of the titrant, follow HI8001EN 5mg/mL Stdz w/
water std or HI8011EN 5mg/mL Stdz w/tartrate.
• Dispense enough methanol from the solvent bottle
to fill the vessel to the “min” line (about 50 mL).
• Press
to pre-titrate the solvent and the titration
vessel moisture. Allow the background drift rate to
stabilize before proceeding to the next step.
ANALYSIS
• Fill the syringe and needle with sample.
• Weigh the syringe, needle and shampoo.
• Press
. You will be prompted to enter the
sample size.
• Dispense 0.015 g to 0.020 g of shampoo into the
titration vessel through the septum using the needle.
• Pay attention not to get any sample on the electrode
or beaker wall. If necessary, swirl the titration
vessel gently by hand to remove any sample on the
electrode or beaker wall.
• Clear the needle of residual sample by intaking a
small volume of air from the titration vessel. If a
“hanging drop” of sample is seen on the end of
the needle, dip the end of the needle briefly in the
solvent.
• Remove the needle from the titration vessel and
weigh the syringe again in order to determine
the added sample mass (by difference of the two
measurements.)
• Use the numeric keypad to enter the exact weight
and press
to start the analysis.
• At the end of the titration the Result screen is
displayed. The results are expressed in % mass of
water.
Name:
Moisture in Shampoo
Method Revision:
1.1
Type:
Sample Analysis
Predispensing Amount:
40 %
Pre-Analysis Stir Time:
15 Sec
Stirring Speed:
900 RPM
Stirbar Type:
Medium
Drift Entry:
Automatic
Solvent:
Methanol
Sample Parameters:
Sample Determ.:
Normal
Sample Name:
Shampoo
Sample Type:
Mass
Sample Size:
0.0200 g
Titrant:
Composite 5
Titrant Type:
one-component
Nominal Titrant Conc.: 5.0000 mg/mL
Std. Titrant Conc.:
5.0000 mg/mL
Date/Time:
Apr 02, 2019 11:45
Titrant Age Reminder:
2d:00h:00m
Control Parameters:
Start Mode:
Normal
Standby Mode:
Enabled
Standby Duration:
12:00 [hh:mm]
Imposed Current:
20 μA
Minimum Dose:
0.500 μL
Maximum Dose:
20.000 μL
Max Dosing Mode
Disabled
Timed Increment:
1 second
End Point Value:
180.0 mV
Signal Averaging:
3 Readings
Flow Rate:
10.0 mL/min
Termination Parameters:
Maximum Duration:
600 sec
Maximum Titrant Volume: 10.000 mL
Term. Criterion:
Relative Drift
Relative Drift:
10.0 μg/min
Result Unit:
%
Significant Figures
XXXXX
Titrant units:
mg/mL
Titrant volume consumed:
V (mL)
Final results units:
% Mass
Titrant concentration: 5.0000 mg/mL
Sample mass:
0.0200 g
RESULTS
Method Name:
Moisture in Shampoo
Time & Date:
Apr 03, 2019 12:00
Sample Size:
0.0200 g
Std. Titrant Conc.:
5.0000 mg/mL
Drift Value:
5.4 μg/min
End Point Volume:
3.2010 mL
Result:
79.8207 %
Titration Duration:
7:19 [mm:ss]
Estimated Cell Volume:
106.37 mL
Titration went to Completion
Operator Name:
Analyst Signature:____________________
3
HI8201EN
CALCULATIONS
APPLICATIONS
METHOD PARAMETERS
3-27
HI8202EN
APPLICATIONS
3
3-28
HI8202EN MOISTURE DETERMINATION IN HAND CREAM
DESCRIPTION
Method for the determination of moisture in hand cream.
The results are expressed in % mass and should be
between 50 and 75 %.
ELECTRODE
• HI76320 Dual Platinum Pin Electrode
REAGENTS
• 5 mg/mL one-component Karl Fischer volumetric
titrant
• Dry methanol
• Dry chloroform
ACCESSORIES
• 1 mL syringe (clean and dry)
• 18-gauge, 6” non-coring septum penetration needle
(clean and dry)
• Solvent bottle, GL45 thread
SOLVENT PREPARATION
• Prepare at least 200 mL of solvent by adding 2
part dry chloroform and 1 part dry methanol to the
solvent bottle.
DEVICE PREPARATION
• Connect the solvent bottle top assembly to the bottle
of solvent according to the manual.
• Assemble the titration vessel according to the
instruction manual.
• Install a 5 mL burette filled with 5 mg/mL onecomponent Karl Fischer volumetric titrant and verify
that no air bubbles are present in the burette or
tubing. If necessary, prime until all air has been
removed completely.
• Press
from the main screen. Use the arrow
keys to highlight HI8202EN Moisture in Hand Cream
and press
.
• For the determination of the exact concentration
of the titrant, follow HI8001EN 5mg/mL Stdz w/
water std or HI8011EN 5mg/mL Stdz w/tartrate.
• Dispense enough solvent from the solvent bottle to
fill the vessel to the “min” line (about 50 mL).
• Press
to pre-titrate the solvent and the titration
vessel moisture. Allow the background drift rate to
stabilize before proceeding to the next step.
ANALYSIS
• Fill the syringe and needle with sample.
• Weigh the syringe, needle and hand cream.
• Press
. You will be prompted to enter the
sample size.
• Dispense 0.020 g to 0.025 g of hand cream into the
titration vessel through the septum using the needle.
• Pay attention not to get any sample on the electrode
or beaker wall. If necessary, swirl the titration
vessel gently by hand to remove any sample on the
electrode or beaker wall.
• Clear the needle of residual sample by intaking a
small volume of air from the titration vessel. If a
“hanging drop” of sample is seen on the end of
the needle, dip the end of the needle briefly in the
solvent.
• Remove the needle from the titration vessel and
weigh the syringe again in order to determine
the added sample mass (by difference of the two
measurements.)
• Use the numeric keypad to enter the exact weight
and press
to start the analysis.
• At the end of the titration the Result screen is
displayed. The results are expressed in % mass of
water.
Name:
Moisture in Hand Cream
Method Revision:
1.1
Type:
Sample Analysis
Predispensing Amount:
40 %
Pre-Analysis Stir Time:
15 Sec
Stirring Speed:
900 RPM
Stirbar Type:
Medium
Drift Entry:
Automatic
Solvent:
CHCl3 MeOH 2:1
Sample Parameters:
Sample Determ.:
Normal
Sample Name:
Hand Cream
Sample Type:
Mass
Sample Size:
0.0200 g
Titrant:
Composite 5
Titrant Type:
one-component
Nominal Titrant Conc.: 5.0000 mg/mL
Std. Titrant Conc.:
5.0000 mg/mL
Date/Time:
Apr 02, 2019 11:45
Titrant Age Reminder:
2d:00h:00m
Control Parameters:
Start Mode:
Normal
Standby Mode:
Enabled
Standby Duration:
12:00 [hh:mm]
Imposed Current:
20 μA
Minimum Dose:
0.500 μL
Maximum Dose:
20.000 μL
Max Dosing Mode
Disabled
Timed Increment:
1 second
End Point Value:
180.0 mV
Signal Averaging:
3 Readings
Flow Rate:
10.0 mL/min
Termination Parameters:
Maximum Duration:
900 sec
Maximum Titrant Volume: 10.000 mL
Term. Criterion:
Relative Drift
Relative Drift:10.0 μg/min
Result Unit:
%
Significant Figures
XXXXX
Titrant units:
mg/mL
Titrant volume consumed:
V (mL)
Final results units:
% Mass
Titrant concentration: 5.0000 mg/mL
Sample mass:
0.0200 g
RESULTS
Method Name:
Moisture Hand Cream
Time & Date:
Apr 03, 2019 12:00
Sample Size:
0.0244 g
Std. Titrant Conc.:5.0000 mg/mL
Drift Value:
5.4 μg/min
End Point Volume:
3.2915 mL
Result:
67.3125 %
Titration Duration:
6:48 [mm:ss]
Estimated Cell Volume:
53.47 mL
Titration went to Completion
Operator Name:
Analyst Signature:____________________
3
HI8202EN
CALCULATIONS
APPLICATIONS
METHOD PARAMETERS
3-29
3
HI8301EN MOISTURE DETERMINATION IN SOLVENT WITH 5 mg/mL TITRANT (ONE-COMP.)
HI8301EN
APPLICATIONS
For External Dissolution or Extraction
3-30
DESCRIPTION
Method for the determination of moisture in extraction/
dissolution solvent using 5 mg/mL one-component Karl
Fischer volumetric titrant. The results are expressed in
% mass and should be less than 0.1%.
ELECTRODE
• HI76320 Dual Platinum Pin Electrode
REAGENTS
• 5 mg/mL one-component Karl Fischer volumetric
titrant
• Dry methanol
ACCESSORIES
• 1 mL syringe (clean and dry)
• 18-gauge, 6” non-coring septum penetration needle
(clean and dry)
• Solvent bottle, GL45 thread
TITRATION PROCEDURE
• Connect the solvent bottle top assembly to the bottle
of methanol according to the manual.
• Assemble the titration vessel according to the
instruction manual.
• Install a 5 mL burette filled with 5 mg/mL onecomponent Karl Fischer volumetric titrant and verify
that no air bubbles are present in the burette or
tubing. If necessary, prime until all air has been
removed completely.
• Press
from the main screen. Use the arrow
keys to highlight HI8301EN Solvent w/ 5mg/mL
1-comp and press
.
• For the determination of the exact concentration
of the titrant, follow HI8001EN 5mg/mL Stdz w/
water std or HI8011EN 5mg/mL Stdz w/tartrate.
• Dispense enough methanol from the solvent bottle
to fill the vessel to the “min” line (about 50 mL).
• Press
to pre-titrate the methanol and the
titration vessel moisture. Allow the background drift
rate to stabilize before proceeding to the next step.
ANALYSIS
• Stop stirring the solvent in the extraction/dissolution
bottle.
• Fill the syringe and needle with the extraction/
dissolution solvent.
• Weigh the syringe, needle and solvent.
• Press
. You will be prompted to enter the
sample size.
• Dispense 0.750 g to 1.000 g of solvent into the
titration vessel through the septum using the needle.
• Pay attention not to get any solvent on the electrode
or beaker wall. If necessary, swirl the titration
vessel gently by hand to remove any sample on the
electrode or beaker wall.
• Clear the needle of residual solvent by intaking a
small volume of air from the titration vessel. If a
“hanging drop” of solvent is seen on the end of
the needle, dip the end of the needle briefly in the
titration solvent.
• Remove the needle from the titration vessel and
weigh the syringe again in order to determine
the added sample mass (by difference of the two
measurements.)
• Use the numeric keypad to enter the exact weight
and press
to start the analysis.
• At the end of the titration the Result screen is
displayed. The results are expressed in % mass of
water. Record this value as the “External Solvent
Concentration”.
METHOD PARAMETERS
5.0000 × V
�
� - 0.0100
40.000
0.7500
× 10
Titrant
units:
mg/mL
Mass =
×
× 100
5.0000
× VV (mL)
3.000
Titrant
volume 100
consumed:
-�
�
Final results units: 0.7500 × 10% Mass
Titrant concentration: 5.0000 mg/mL
Sample mass:
1.0000 g
% Mass =
V × 5.0000
1.0000 × 10
RESULTS
3
APPLICATIONS
Method Name: Solvent w/ 5mg/mL 1-comp.
Time & Date:
Apr 03, 2019 12:00
Sample Size:
0.9580 g
Std. Titrant Conc.:
5.0000 mg/mL
Drift Value:
4.0 μg/min
End Point Volume:
0.1157 mL
Result:
0.0595 %
Titration Duration:
2:06 [mm:ss]
Estimated Cell Volume:
57.5 mL
Titration went to Completion
Operator Name:
Analyst Signature:____________________
HI8301EN
Name:
Solvent w/ 5mg/mL 1-comp.
%
Method Revision:
1.1
Type:
Sample Analysis
Predispensing Amount:
None
Pre-Analysis Stir Time:
0 Sec
Stirring Speed:
900 RPM
Stirbar Type:
Medium
Drift Entry:
Automatic
Solvent:
Methanol
Sample Parameters:
Sample Determ.:
Normal
Sample Name:
Solvent
Sample Type:
Mass
Sample Size:
1.0000 g
Titrant:
Composite 5
Titrant Type:
one-component
Nominal Titrant Conc.: 5.0000 mg/mL
Std. Titrant Conc.:
5.0000 mg/mL
Date/Time:
Apr 02, 2019 11:45
Titrant Age Reminder:
2d:00h:00m
Control Parameters:
Start Mode:
Cautious
Standby Mode:
Enabled
Standby Duration:
12:00 [hh:mm]
Imposed Current:
20 μA
Minimum Dose:
0.250 μL
Maximum Dose:
5.000 μL
Max Dosing Mode
Disabled
Timed Increment:
1 second
End Point Value:
180.0 mV
Signal Averaging:
3 Readings
Flow Rate:
10.0 mL/min
Termination Parameters:
Maximum Duration:
600 sec
Maximum Titrant Volume:
5.000 mL
Term. Criterion:
Relative Drift
Relative Drift:
10.0 μg/min
Result Unit:
%
Significant Figures
XXXXX
CALCULATIONS
3-31
PART 4:
TITRATION THEORY
TITRATION THEORY
4
TITRATION THEORY
4
1. TITRATION THEORY
1.1. INTRODUCTION TO TITRATIONS
A titration is a quantitative, volumetric procedure used in analytical chemistry to determine the concentration of an
analyte (the species being measured) in solution. The concentration of the analyte is determined by slowly adding a
titrant (reagent) to the solution. As the titrant is added, a chemical reaction occurs between the titrant and the analyte.
Titration reactions are relatively fast, simple reactions that can be expressed using a chemical equation. The titration
reaction continues as the titrant is added until all of the analyte is consumed and the analyte reacts completely and
quantitatively with the titrant.
The point at which all of the analyte has been reacted is called the equivalence point, also known as the theoretical or
stoichiometric end point. This point is accompanied by an abrupt physical change in the solution, which sharply defines
the end point of the reaction. The physical change associated with the titration end point can be produced by the titrant
or an indicator, and can be detected either visually or by some other physical measurement.
Titrations cannot be used to determine the quantity of all analytes. The chemical reaction between the titrant and analyte
must fulfill four requirements:
• The reaction must be fast and occur within approximately one second after the titrant has been added
• The reaction must go to completion
• The reaction must have well-known stoichiometry (reaction ratios)
• A convenient end point or inflection point
Titrations are highly precise and can provide many advantages over alternative methods. Titrations are quickly performed
and require relatively simple apparatus and instrumentation.
1.2. USES OF TITRATIONS
Titrations can be used in many applications, including:
• Acid content of plant effluents, food (e.g. cheese and wine), plating and etching baths, petroleum products, drugs
• Base content of fertilizer (containing ammonia), bleach, minerals
• Hardness in water
• Metal content of alloys, minerals, ores, clays, waters, plating baths, paints, paper, plant materials, biological
fluids, petroleum products
• Moisture content in foodstuff, petrochemicals, pharmaceutical products, and plastics
• Redox reagent concentrations such as available chlorine in potable water, peroxide, traces of oxidants and
reductants in food, reductants in high temperature or high pressure boiler water, vitamin analysis
1.3. ADVANTAGES AND DISADVANTAGES OF TITRATIONS
Some advantages of titrations as an analytical technique are:
• More precise results than many instrumental methods, such as measurement by electrode, the accuracy of the
measurement is up to 0.1%
• Simple methods, reasonable capital costs, and easy training
• Suitability to measure major components of a mixture or product
• Automation can reduce time and labor spent on each analysis
Some disadvantages of titrations are:
• The time it takes to prepare standards and titrants
• Good technique is required to achieve precise results (training and practice required)
• Not suitable for determining trace or minor components of a mixture or product
• Limited dynamic range, it may require additional sample preparations (dilution) and repeat analyses
4-2
4
2. TYPES OF TITRATIONS
2.1. TITRATIONS ACCORDING TO THE MEASUREMENT METHOD
TITRATION THEORY
2.1.1. AMPEROMETRIC TITRATIONS
An amperometric titration is performed by placing two electrodes (often a metal ion selective electrode and a reference
electrode) into the sample solution and keeping the potential of the metal electrode at a selected voltage. The current
that flows, due to the oxidation or reduction of a reactant or product, is plotted vs. volume of titrant to provide the
titration curve and locate the equivalence point. Changes in the current are due to changes in the concentration of a
particular species (being oxidized or reduced at the electrode).
Generally the reaction between the analyte and titrant forms a new species. Depending on the titration, the reactants
are electroactive and the products are not, or vice-versa. Amperometric titration curves look like two straight lines
intersecting at the equivalence point, this is due to the change in the electroactivity of the solution.
Many metal ions can be amperometrically titrated using a precipitation, complexation or redox reaction. Some metal ions
and species that can be determined in this manner include silver, barium, halides, potassium, magnesium, palladium,
molybdate, sulfate, tungstate, zinc, bismuth, cadmium, fluoride, indium, thallium, iodine, and gold.
Figure 1 shows four amperometric titrations and their end points. In graph A the analyte is electroactive and gives
current but the reacted species does not. In B the reactant is not active but the titrant is. In C both the analyte and titrant
are active and both give current flow. Graph D shows the same situation as B; however, the current has an opposite sign
(the titrant is reduced).
Figure 1
2.1.2. POTENTIOMETRIC TITRATIONS
Potentiometric titrations are done by measuring the voltage across the solution using an electrode system. An electrode
system consists of an indicator electrode and a reference electrode. As titrant is added, the variations in the potential
of the indicator electrode, with respect to the reference electrode, are monitored to show the progress of the titration.
Potentiometry is the measurement of a potential under conditions of zero current flow. The measured potential can then
be used to determine the analytical quantity of interest, generally a component concentration of the analyte solution.
4-3
TITRATION THEORY
4
The potential that develops in the electrochemical cell is the result of the free energy change that would occur if the
chemical phenomena were to proceed until the equilibrium condition has been satisfied.
There are many types of titrations where potentiometry can be used, e.g. pH electrodes for acid-base titrations, platinum
ORP electrodes in redox titrations, ion selective electrodes, such as chloride or fluoride for a specific ion titration, and
silver electrodes for argentometric (silver-based) titrations.
2.1.3. SPECTROPHOTOMETRIC TITRATIONS
The name comes from the method used to detect the end point of the titration, not its chemistry. Highly colored indicators
that change color during the course of the titration are available for many titrations. More accurate data on the titration
curve can be obtained if the light absorption is monitored instrumentally using a light source, a simple monochromator
and a photodetector, rather than visually determining the color or light absorption change. Light absorption by either an
indicator or by one of the reactants or products can be used to monitor the titration.
Figure 2, shows two titration curves. In graph A the absorption of a metal-indicator complex is being monitored. The
absorption is constant while the metal is complexed by the EDTA titrant. The metal indicator complex was stripped,
causing a sharp break in the titration curve. The point where all the metal is complexed and stripped from the indicator
is the equivalence point. This point is marked by “e.p.” on the graph.
In the second titration curve, graph B, the metal complex is being measured while being titrated with EDTA. The new
complex being formed is not colored and does not absorb light. The extrapolated intersection of the two lines determines
the equivalence point.
Figure 2
2.2. TITRATIONS ACCORDING TO THE REACTION TYPE
2.2.1. KARL FISCHER TITRATIONS
This method is based on a well-defined chemical reaction between water and the Karl Fischer reagent. The chemistry
provides excellent specificity for water determination. The method can be used to determine free and bound water in a
sample matrix. The Karl Fischer method is widely considered to produce the most rapid, accurate and reproducible results
and has the largest detectable concentration range spanning 1 ppm to 100%.
The determination of water content is one of the most commonly practiced methods in laboratories around the world.
Knowledge of water content is critical to understanding chemical and physical properties of materials and ascertaining
product quality. Water content determination is conducted on many sample types including pharmaceuticals and
cosmetics, foods and natural products, organic and inorganic compounds, chemicals, solvents and gases, petroleum and
plastic products as well as paints and adhesives. The KF method is verifiable and can be fully documented. As a result,
Karl Fischer titration is the standard method for analysis of water in a multitude of samples as specified by numerous
organizations including the Association of Official Analytical Chemists, the United States and European Pharmacopoeia,
ASTM, American Petroleum Institute, British Standards and DIN.
4-4
4
TITRATION THEORY
2.2.1.1. HISTORY OF KARL FISCHER TITRATIONS
Water determination by Karl Fischer titration is based on the reaction described by Bunsen in 1853 in which sulfur
dioxide is oxidized by iodine in the presence of water.
I2 + SO2 + 2 H2O → 2 HI + H2SO4
In Karl Fischer’s 1935 article, “a new procedure for the titration of water”, he presented a modified form of the Bunsen
reaction adapted for use in determining the water content of non-aqueous solutions. His titrations were conducted in
methanol in the presence of excess sulfur dioxide and pyridine in order to neutralize the acidic reaction products and
drive the reaction to completion.
2 H2O + SO2 • (C5H5N)2 + I2 + 2 C5H5N → (C5H5N)2 • H2SO4 + 2 C5H5N • HI
Two key developments have since lead to the currently accepted description of the Karl Fischer reaction. First, pyridine
acts as a pH buffer and does not play a direct role in the reaction. This has allowed reagent formulators to replace
pyridine with bases which are both less toxic and result in pH ranges that facilitate faster and more accurate titrations.
Second, the species that reacts with water is not sulfur dioxide but the monomethyl sulfite ion resulting from the reaction
between sulfur dioxide and methanol. Subsequently, researchers showed that higher alcohols can be used in place of
methanol. The Karl Fischer reaction can therefore be described by the following generalized reaction sequence in which
the H2O, I2, SO2 and RN species react in a 1:1:1:3 stoichiometry.
ROH + SO2 + RN → (RNH)•SO3R
(RNH)•SO3R + I2 + H2O → (RNH)•SO4R + 2(RNH)I
The maximum rate of the Karl Fischer reaction is reached between the pH range of 5.5 to 8 where all of the sulfur
dioxide is available as methyl sulfite. If the pH drops below 5, the rate of reaction decreases and titration end point
become increasingly difficult to reach. If the pH exceeds 8, side reactions begin to occur between iodine and hydroxide
or methylate ions, changing the titration stoichiometry.
While solvents not containing alcohols can be used for Karl Fischer analysis, they also have an effect on reaction
stoichiometry. When alcohols are not present, the reaction resembles the Bunsen reaction stoichiometry where the
consumption ratio of water to iodine is 2:1. In solvents containing higher alcohols, uneven ratios can be observed due
to the relative abilities of higher alcohols to form the sulfite ester that reacts with water. Issues resulting from solventinduced variation in stoichiometry are not typically encountered during routine analysis for two reasons. First, titrant
standardization and sample analysis are carried out in the same titration medium and under the same conditions,
effectively compensating for any variation in reaction behavior. Second, most Karl Fischer reagent systems are formulated
to support standard KF reaction stoichiometry.
2.2.1.2. VISUAL INDICATION OF KARL FISCHER TITRATIONS
Visual methods, originally used by Karl Fischer, are limited in application, require a high degree of skill and have
been made obsolete by electrometric indication. For successful visual indication, titration samples must be colorless.
Additionally, the solution coloration varies between polar and non-polar titration media.
After the titration equivalence point, all of the water in the titration solution has been reacted. The next drop of titrant,
added to the solution after the equivalence point, contains iodine that will remain in the titration solution. Thereafter,
the concentration of iodine in the titration solution increases and the solution develops a yellow, and eventually brown,
color. It is difficult, even for an experienced analyst, to generate reproducible end point coloration between successive
titrations.
4-5
TITRATION THEORY
4
2.2.1.3. ELECTROMETRIC INDICATION OF KARL FISCHER TITRATIONS
Biamperometric and bivoltametric indication are the two types of electrometric detection methods commonly used for
indication of Karl Fischer titrations. Both methods use either a double platinum pin or a double platinum ring electrode
to detect excess iodine in a titration solution. After the titration equivalence point, all of the water in the titration solution
has been reacted. The next dose of titrant added to the solution contains iodine, which reacts at the electrode according
to the reactions below.
At the cathode: I2 + 2e-→ 2IAt the anode:
2I-→ I2 + 2eThe excess iodine is easily reduced at the cathode, and the resulting iodide is oxidized at the anode.
Both electrometric methods of indication rely on electrons (current) being carried through a titration solution by the
oxidation-reduction reactions described above. Biamperometric indication involves monitoring the flow of current
through the titration solution while a constant voltage is applied across the platinum elements of the electrode. When
water is present in the titration solution and there is no excess iodine, only minimal current flows between the electrode
elements. After the equivalence point, when iodine is present, the current flow increases to a few μA.
Bivoltametric indication involves measuring the voltage required to maintain a constant current flow between electrode
elements. A small direct or alternating current called a polarization current (Ipol) is applied between the electrode pins or
rings, and the resulting voltage is measured in order to monitor the titration progress.
L-shaped titration curves are generated for both methods by plotting either the electrode current or voltage against the
volume of titrant added during the titration.
Figure 3
Electrometric methods result in over-titration or titration past the equivalence point, where excess iodine is present in
the titration solution. Titration past the equivalence point is acceptable for two reasons. First, due to the sensitivity of
the electrometric methods, titrations are always carried out exactly the same, slight excess of iodine resulting in highly
reproducible titrations. Second, the accuracy of electrometrically indicated titrations are not affected by the over-titration
because the slight excess of iodine has been accounted for during the standardization of the titrant.
4-6
4
TITRATION THEORY
2.2.2. ACID-BASE TITRATIONS
Acid-base titrations are the most common type of titrations. Acid-base titrations are based upon a reaction between an
acid and a base, a stoichiometric neutralization, or the exchange of protons. Virtually all acid-base titrations are carried
out using a strong acid or a strong base as the titrant. The end point of a titration carried out with a weak acid or a weak
base, would be difficult to detect due to a small change in pH at the equivalence point.
Chemical indicators are often used to determine the end point. The indicator will change color to signify that the end of
the titration has been reached. When choosing the proper indicator you should select one that has a pKa as close to the
end point of the titration as possible. The color-change region of the indicator is usually ± 1 pH unit around the pKa.
The theoretical titration curve is useful for illustrating how the solution will change during the real titration, and allowing
the proper selection of an end point or an indicator.
Figure 4 shows a traditional titration curve. The curve is obtained by plotting the pH value against the volume of NaOH
added.
Figure 4
4-7
TITRATION THEORY
4
2.2.3. ARGENTOMETRIC TITRATIONS
Argentometric titrations use silver (nitrate) as the titrant and are generally precipitation titrations, as many silver salts
are insoluble. These titrations are commonly used to titrate and determine the concentration of bromide, chloride,
cyanide, iodide, and sulfide.
Argentometric titrations can be done with Mohr’s indicator. After all of the chloride has reacted, a red silver chromate
precipitate is formed or the titration can be easily followed with a silver ISE (or chloride ISE for chloride titrations) and
a reference electrode.
Figure 5
Figure 5 shows the titration of 50 mL of 0.1N NaCl with 0.1N AgNO3. The potentiometric signal is from a chloride ISE,
and is plotted as pCl (- log [Cl-]).
2.2.4. COMPLEXOMETRIC TITRATIONS
A complex is a species where a central metal ion is covalently bonded to one or more electron donating groups called
ligands. In a complexometric titration, metal ions are titrated using a titrant that binds strongly to it. Often these
titrants contain EDTA or CDTA, polydentate ligands that form very stable coordination compounds with metal ions. The
complexation reaction must be fast in order to be useful for direct titration. Some metal ions react too slowly with EDTA
for a direct titration.
An indicator electrode that responds to the metal ion can be used to monitor the titration progress. The titration curve
will appear similar to a usual potentiometric titration. Complexation indicators change color at the end point as all metal
ions are “consumed”, or complexed by the titrant.
The titration curve will appear similar to a potentiometric titration, when using an indicator electrode that responds to
the metal ion (see Figure 6).
4-8
4
TITRATION THEORY
Figure 6
2.2.5. ION SELECTIVE TITRATIONS
The most popular ion selective titration is an acid-base titration. The hydrogen ion concentration is specifically measured
and monitored during the titration process to locate the equivalence point. Using an ion selective electrode (ISE) as the
indicator electrode, the potentiometric signal (in mV) is used to directly follow a specific ion’s concentration (or activity).
Examples of ISE titrations include titrating fluoride with an aluminum titrant using a fluoride ISE, chloride with silver
nitrate using a chloride ISE, sodium with a sodium ISE, etc. The equivalence point can be determined by plotting the
mV value vs. the amount of titrant added.
2.2.6. NON-AQUEOUS SOLVENT ACID-BASE TITRATIONS
Non-aqueous solvents must be used to titrate very weak acids and bases due to the inherent leveling effect water has on
all acids and based dissolved in it. A wide variety of weak acids and bases can be titrated using non-aqueous solvents.
Mixtures of acids or bases can often be individually analyzed in a single sequential titration.
2.2.6.1. TITRATION OF ACIDS
Weak acids with pKa’s up to about 11 can be titrated in non-aqueous solvents. These include carboxylic acids, enols,
phenols, imides, sulfonic acids, and inorganic acids. Water or lower alcohols are suitable for titrating medium to strong
acids (pKa less than 5). Titrating a weaker acid with a strong base titrant requires a solvent less acidic than water
or ethanol/methanol. Solvents such as acetone, acetonitrile, t-butyl alcohol, dimethlyformamide, isopropanol and
pyridine have been found to work well for acid-base titrations of strong, medium and weak acids/bases. Titrants include
alcoholic potassium hydroxide and various sodium or potassium alkoxides in a 10:1 mixture of benzene/methanol. The
best titrants are quaternary ammonium hydroxides (such as tetrabutylammonium hydroxide) due to good solubility of
tetraalkylammonium salts of the titrated acids and the clean potentiometric titration curve obtained (see Figure 7)
4-9
TITRATION THEORY
4
2.2.6.2. TITRATION OF BASES
Weak bases with pKb’s up to about 11, which do not ionize with water, can be titrated in non-aqueous solvents. These
bases include aliphatic and aromatic amines, basic nitrogen heterocycles, alkali metal and amine salts of acids, and
many other organic basic compounds. Titrating a weak base with a strong acid titrant requires a basic solvent that is as
weak as possible. Water and alcohols allow the titration of medium strength bases such as aliphatic amines (pKb = 4
to 5), but not the titration of weaker bases such as pyridine (pKb = 8.8). Glacial acetic acid works well for weak bases
and has been used extensively. Less basic solvents such as acetone, acetonitrile, and nitromethane extend the range of
titrable compounds.
The end point for non-aqueous titrations are usually determined potentiometrically using a pH glass electrode, a
modified calomel or double junction reference electrode with a low-flow rate reference junction. Good potentiometric
titration curves are obtained in most solvents, except those with very low dielectric constants such as benzene, chloroform
and others, when high electrical resistance of the solvent causes unstable potentials.
2.2.7. PRECIPITATION TITRATIONS
Precipitation titrations allow for faster analysis compared to the old gravimetric analysis, where a precipitate is formed,
filtered, dried and weighed to analyze a compound. Typically silver halides, silver thiocyanate and a few mercury, lead,
and zinc salts are titrated using this method. The chemical reactions must form an insoluble salt and precipitate out
quickly in order to be analyzed by this method. When the reaction is not quick, a back titration can be used. A measured
excess of the precipitating reagent (titrant) is added to force the reaction to occur, and then unreacted titrant is titrated
with a standard solution of another reagent.
2.2.8. REDOX TITRATIONS
There are a number of oxidation-reduction reactions that can be used to determine unknown concentration by titration. If
the reaction goes to completion, is fast and has an analytical signal available to follow it, a titration can be performed.
The term “fast” means that each addition of titrant is reacted completely and the sensing electrode is able to detect the
change in solution in less than one second (see Figure 8).
Redox titrations are potentiometric titrations where the mV signal from a combination ORP (redox) electrode (usually
with a platinum indicator electrode) is used to follow the reaction of oxidant/reductant. The electrode potential is
determined by the Nernst equation and is controlled by the oxidant reductant ratio.
Figure 7
4-10
Figure 8
2.3. TITRATIONS ACCORDING TO THE TITRATION SEQUENCE
2.3.1. BACK TITRATIONS
Back titrations are generally used when a reaction is too slow to be directly accomplished during a “direct” titration,
where the reaction goes to completion within a few seconds. In a back titration, a large excess of a reagent is added
to the sample solution, helping a slow reaction to go to completion. The unreacted, excess reagent is then titrated. The
difference in the total volume of the first reagent added and amount determined from the second titration is the quantity
of reagent required to complete the first reaction.
4
TITRATION THEORY
Visual indicators such as Ferroin are also available. The oxidized and reduced form of the indicator will have different
colors and can be used to determine the end point.
Various reductants can be determined by titrants with oxidants such as potassium permanganate, potassium chromate
or iodine. Commonly used reductants that are used as titrants include sodium thiosulfate and ferrous ammonium sulfate.
As with Acid-Base titrations the potential changes dramatically at the equivalence point.
2.3.2. MULTIPLE END POINT TITRATIONS
Under certain conditions, some titrations can exhibit more than one equivalence point and be titratable to the individual
end points to determine the concentration of each individual component. Examples of these types of titrations include
acid-base, where different strength acid or bases are in a mixture; redox, where each species has a different reduction
potential; complexometric, where different species are separately titratable; and acid-base, using polyprotic acids (the
pKa of the different protons varies enough to separate them).
Figure 9 shows three different types of multiple end point titrations. Graph A shows the titration of a polyprotic acid. The
different acid strengths of the first and second proton can be determined. Graph B illustrates a mixture of two different
metal redox species, where the different redox potentials allow the species to be separated. Graph C is the titration of a
solution containing strong, weak, and very weak acids.
A
B
C
Figure 9
4-11
4
3. TITRATION PROCEDURE
TITRATION THEORY
3.1. MANUAL TITRATION
Apparatus required for manual titration include:
• Volumetric burette, for precisely controlled delivery of titrant to the reaction vessel
• An Erlenmeyer, or similar flask, that facilitates constant mixing or swirling required to ensure solution homogeneity
• Volumetric pipettes for the precise addition of samples and indicator solutions
• Titrant solutions of known concentration
• A visual or instrumental indicator for detecting the completion of the reaction
A typical manual titration consists of the following steps:
1) A volumetric pipette is typically used to add a known volume of sample to the flask.
2) An indicator solution or instrument probe is added to the flask.
3) A burette is used to measure the addition of titrant to the flask and dispense titrant in a controlled manner.
4) Titrant is added via the burette until the method indication signals the reaction end point.
5) The concentration of analyte is calculated based on the concentration and volume of titrant required to reach the
end point.
Wrap fingers around tap, keeping
pressure on to stop tap coming out
Swirl flask constantly
3.2. AUTOMATIC TITRATION
4-12
Automatic titrators are high-precision analytical instruments that deliver the titrant, monitor the physical change
associated with the titration reaction, automatically stops at the end point and calculates the concentration of the
analyte. Automatic titrators are best for repetitive titrations and high-accuracy analyses.
An automatic titrator must have an accurate liquid dispensing system. In high accuracy systems like the HI900-series
titrators, the liquid dispensing system consists of a stepper-motor driven piston syringe burette capable of accurately
and precisely dispensing very small volumes of titrant, a valve system to switch between titrant intake and outlet, and a
dispensing tip. These three main subsystem components must be as accurate as possible, with very low gear backlash in
the burette pump, minimal piston seal flexing, precision ground inner diameter of the glass syringe, a low dead volume
valve, minimal evaporation/permeation, and chemically resistant tubing.
4
TITRATION THEORY
Apparatus required for automatic titration include:
• An automatic titrator, equipped with a burette
• A beaker
• An electronic stirring system, either a propeller stirrer or a magnetic stir bar and stir plate
• Volumetric pipettes for the precise addition of samples
• Standard titrant solutions of known concentration
• An electrode system that can be used to determine the end point of the titration
A typical automatic titration consists of the following steps:
1) Set up the automatic titrator according to the manufacturer’s instructions.
2) A volumetric pipette is typically used to add a known volume of sample to the beaker.
3) Submerge the propeller stirrer or add the stir bar to the beaker and turn on.
4) Start the titration, the titrator will automatically stop at the end point and determine the concentration of the
analyte.
4-13
4
4. TITRATION RESULTS
TITRATION THEORY
4.1. ACCURACY
The factors most critical to achieving accurate results with the HI900 titration systems are the concentration of the
sample, size of the sample and having an optimized set of method parameters.
4.2. REPEATABILITY
Repeatability, or the agreement between replicate determinations, is expressed quantitatively as the relative standard
deviation (RSD).
4.3. SOURCES OF ERROR
One of the advantages of volumetric analysis is excellent accuracy and precision. The sources of error can be grouped into
sampling, titrant and standards, chemical reactions, end point determination and calculations.
4.3.1.
•
•
•
•
SAMPLING ERRORS
Selection of a non-homogeneous or non-representative sample
Sample changed or was contaminated during collection, storage or transfers
Poor technique when transferring sample to beaker or flask
Errors in the balance (calibrate and check balance regularly)
4.3.2. PREPARATION ERRORS
Incorrect preparation due to:
• Poor technique in weighing the salt or when transferring to volumetric glassware
• Low-purity of salts or water used to make titrant and standard
• Dirty or wet glassware
• Improper storage of titrant or standard which allows water gain, evaporation or deterioration
• Failure to standardize frequently to adjust for change in titrant
• Failure to flush titrator tubing with a volume of titrant before standardizing
• Volume errors from pipettes and volumetric flasks (grade A glassware is required)
• Balance errors when weighing out salts (calibrate and check balance regularly)
4.3.3. DISPENSING ERRORS
Incorrect dispensing due to:
• Dead valve volume and leaking valve
• Inaccuracy in motor drive and gear lash/backlash
• Poor burette/piston seal
• Non-uniform diameter of burette glass cylinder
• Chemical incompatibility with tubing or bubble generation
• Density/temperature changes in titrant
• Inadequate volume to cover electrode
4-14
CHEMICAL REACTION ERRORS
Inappropriate solvent or sample, resulting in side reactions
Poor mixing of the titrant and solvent or sample in the titration vessel
Reaction between titrant and sample is not rapid
Reaction does not go to completion
Reaction has side reactions
4.3.5. END POINT DETERMINATION ERRORS
Most manual titrations use a visual indicator to indicate when the end point is reached and the titration should be
stopped. Automatic titrators use instrumental methods to determine the end of a titration and the equivalence point.
There are two predominant methods used to determine the equivalence point, first derivative and second derivative.
The inflection point of the titration curve (mV vs. Volume) is normally assumed to be the equivalence point. The first
derivative is often used to determine the inflection point. The maximum value of the first derivative (∆mV vs. ∆V)
corresponds to the theoretical equivalence point. During a titration it is rare to have a data point exactly at the first
derivative maximum, the maximum value is determined by interpolating the first derivative data points.
The second derivative (∆mV2 vs. ∆V2 ) can also be used to determine the equivalence point, and can offer advantages
over the first derivative method. Second derivatives have increased sensitivity to smaller inflection points and easier
numerical evaluation of the actual equivalence point. The value where the second derivative is equal to zero is the
equivalence point. The second derivative requires fewer points located near the equivalence point, where data is often
not obtained or not as reliable.
Errors in determining the end point can result from:
• Incorrect signals from the sensor
• Sensor drift
• Sensor or instrument has slow response (it is recommended to keep the sensors in good condition)
• Inappropriate setting on the titrator
4
TITRATION THEORY
4.3.4.
•
•
•
•
•
4-15
4
5. CALCULATIONS
TITRATION THEORY
5.1. EQUATIONS USED IN VOLUMETRIC KARL FISCHER TITRATIONS
5.1.1. CALCULATION OF WATER CONTENT AS % MASS FROM SAMPLES MEASURED BY MASS
Csample
Vtitrant
Titer
msample
Concentration of Sample (% w/w)
Volume of Titrant (mL)
Titrant Titer (mg/mL)
Mass of sample (g)
5.1.2. CALCULATION OF WATER CONTENT AS % MASS FROM SAMPLES MEASURED BY VOLUME
Csample
Vtitrant
Titer
Vsample
dsample
Concentration of Sample (% w/w)
Volume of Titrant (mL)
Titrant Titer (mg/mL)
Volume of Sample (mL)
Density of Sample (g/mL)
5.1.3. CALCULATION OF WATER CONTENT AS % VOLUME FROM SAMPLES MEASURED BY VOLUME
Csample
Vtitrant
Titer
Vsample
dwater
Concentration of Sample (% w/w)
Volume of Titrant (mL)
Titrant Titer (mg/mL)
Volume of Sample (mL)
Density of Water at Analysis Temperature (g/mL)
5.1.4. CALCULATION OF WATER CONTENT AS % MASS SUBTRACTING BACKGROUND DRIFT RATE
Csample
Vtitrant
Titer
Drift
t
msample
4-16
Concentration of Sample (% w/w)
Volume of Titrant (mL)
Titrant Titer (mg/mL)
Background Drift Rate (μg/min)
Titration Duration (min)
Mass of Sample (g)
5.1.5. CALCULATION OF WATER CONTENT IN EXTERNAL DISSOLUTION SAMPLES
Concentration of Sample (% w/w)
Mass of Solvent (g)
Water Content of Dissoluted Sample (w/w)
Water Content of Solvent (w/w)
Mass of Sample (g)
5.1.6. CALCULATION OF WATER CONTENT IN EXTERNAL EXTRACTION SAMPLES
Csample
msolvent
Csupernatant
Csolvent
msample
TITRATION THEORY
Csample
msolvent
Csolution
Csolvent
msample
4
Concentration of Sample (% w/w)
Mass of Solvent (g)
Water Content of Dissoluted Sample (w/w)
Water Content of Solvent (w/w)
Mass of Sample (g)
5.1.7. CALCULATION OF WATER CONTENT IN GASEOUS SAMPLES
The water content of gases is normally reported in units of μg/L or mg/L.
Csample
Concentration of Sample (mg/mL)
Vtitrant
Volume of Titrant (mL)
Titer
Titrant Titer (mg/mL)
Flow Rate Sample Flow Rate (L/min)
Flow Duration
Sample Extraction Time (min)
To calculate the water content in %w/w the mass of the gas introduced into the titration vessel must be known. This
can be determined by calculations using ideal gas laws or by measuring the mass of the sample container before and
after a titration.
5.1.8. CALCULATION OF TITER (WATER EQUIVALENT OF THE TITRANT) USING SODIUM TARTRATE
DIHYDRATE CONTAINING 15.66% WATER BY MASS
Ctitrant
msample
Ctartrate
Vtitrant
Titrant Titer (mg/mL)
Mass of Sample (g)
Water Content of Tartrate (156.6 mg/g)
Volume of Titrant (mL)
4-17
TITRATION THEORY
4
5.1.9. CALCULATION OF TITER (WATER EQUIVALENT OF THE TITRANT) USING WATER STANDARDS
Ctitrant
msample
Cstandard
Vtitrant
Titrant Titer (mg/mL)
Mass of Sample (g)
Water Content of Standard (mg/g)
Volume of Titrant (mL)
5.2. EQUATIONS USED IN TITRATIONS
The main variables used in calculating a result from a titration are the sample volume, the concentration of the titrant,
and the volume of titrant required to reach the equivalence point. At the equivalence point, an equal number of
equivalents of the analyte and titrant has been added.
5.2.1. SAMPLE CALCULATION BY MASS
Csample
Vtitrant
Ctitrant
Ratio
FWanalyte
msample
Sample Concentration (g/100g)
Volume of titrant
Titrant Concentration (eq/L)
Equivalence ratio of analyte/ titrant (mol analyte/ eq titrant)
Formula Weight of the Analyte (g/mol)
Mass of sample (g)
5.2.2. SAMPLE CALCULATION BY VOLUME
Csample
Vtitrant
Ctitrant
Ratio
FWanalyte
Vsample
4-18
Sample Concentration (g/100g)
Volume of titrant
Titrant Concentration (eq/L)
Equivalence ratio of analyte/ titrant (mol analyte/ eq titrant)
Formula Weight of the Analyte (g/mol)
Volume of Sample (mL)
Ctitrant
mstandard
Ratio
FWstandard
Vtitrant
Titrant Concentration (N)
Mass of Standard (g)
Equivalence ratio of titrant/standard (eq titrant/ mol standard)
Formula Weight of the Standard (g/mol)
Volume of Titrant (L)
4
TITRATION THEORY
5.2.3. STANDARDIZE TITRANT BY MASS
Titrant standardization is the second most important calculation in titrations. A primary standard is titrated in order
to determine the concentration of the titrant. This is essentially a typical titration calculated in “reverse”, where the
concentration of the solution is known and the titrant is unknown.
5.2.4. STANDARDIZE TITRANT BY VOLUME
Ctitrant
Vstandard
Cstandard
Vtitrant
Titrant Concentration (N)
Volume of Standard (mL)
Concentration of Standard (eq/L)
Volume of Titrant (L)
5.2.5. BLANK TITRATION
In a blank titration a pre-titration is performed, often times on the solvent to be used for the sample titration, and the
titrant volume required to reach the end point is noted. This blank value nullifies error due to titrant required to react with
the components of the titration solution matrix. The basic titration equation can be used for a blank titration, with the
single modification that the volume of titrant used in the blank titration should be subtracted from the regular titration
titrant volume.
Csample
Ctitrant
Vsample
Vblank
Ratio
FWanalyte
msample
Sample Concentration (g/100 g)
Titrant Concentration (eq/L)
Volume of Titrant required for the sample (L)
Volume of Titrant required for the blank (L)
Equivalence ratio of analyte/ titrant (mol analyte/ eq titrant)
Formula Weight of the Analyte (g/mol)
Mass of sample (g)
4-19
TITRATION THEORY
4
5.2.6. MULTIPLE END POINT TITRATION
Some titrations have two or more end points, each corresponding to the equivalence point for a specific reaction. Multiple
end point titrations are similar to a blank titration in that the volume of titrant required to reach the first end point is
subtracted from the titrant volume used to reach the next sequential end point.
Csample1
Csample2
Csample3
Vtitrant 1
Vtitrant 2
Vtitrant 3
Ctitrant
Ratio
FWanalyte 1
FWanalyte 2
FWanalyte 3
msample
Sample 1 Concentration (g/100g)
Sample 2 Concentration (g/100g)
Sample 3 Concentration (g/100g)
Volume of titrant required to reach the first end point (L)
Volume of titrant required to reach the second end point (L)
Volume of titrant required to reach the third end point (L)
Concentration of titrant (N)
Equivalence ratio of analyte/titrant (mol analyte/eq titrant)
Formula Weight of the Analyte 1 (g/mol)
Formula Weight of the Analyte 2 (g/mol)
Formula Weight of the Analyte 3 (g/mol)
Mass of Sample (g)
5.2.7. BACK TITRATION
The equation used in back titration calculations is also similar to the equation for a blank titration. Instead of subtracting
the initial amount of titrant needed to react with the blank, the amount of second titrant needed to react with the excess
titrant added in the first titration is subtracted from the amount of the first titrant added. The difference between the two
amounts is the amount of titrant necessary to reach the first equivalence point.
Csample
Ctitrant 1
Vtitrant 1
Ctitrant 2
Vtitrant 2
Ratio
FWanalyte
Vsample
4-20
Sample Concentration (g/100mL)
Concentration of titrant 1 (N)
Volume of titrant 1 (L)
Concentration of titrant 2 (N)
Volume of titrant 2 (L)
Equivalence ratio of analyte/titrant (mol analyte/ eq titrant)
Formula Weight of the analyte (g/mol)
Volume of sample (mL)
6. GLOSSARY
Acid-Base Titration
Stoichiometric neutralization titrations, based upon the reaction that occurs between an acid and base.
Activity
A physical property corresponding to the concentration of all ions in a solution. Electrodes respond to activity.
Amperometric Titration
Titrations where the current flow between two electrodes (often a metal electrode and a reference electrode) are used to
monitor the titration progress.
TITRATION THEORY
Acid
A chemical species that can donate one or more protons (hydrogen ions).
4
Analyte
The chemical species being measured in a titration.
Argentometric Titration
Titrations that use silver (nitrate) as the titrant. These titrations are typically precipitation titrations.
Automatic Titrator
An instrument designed to automatically carry out a titration. It will add the appropriate amount of titrant, determine
the end-point and calculate the results.
Back Titration
A type of titration where an excess amount of titrant is added to a sample forcing a sluggish reaction to go to completion.
The excess reagent is then “back” titrated with a second titrant.
Base
A chemical species that can accept one or more protons (hydrogen ions).
Biamperometric Indication
Uses a double platinum pin electrode to measure the current flow through a titration solution.
Bivoltametric Indication
Uses a double platinum pin electrode to measure the voltage required to maintain a constant current flow through a
titration solution while constant voltage is applied across the platinum elements of the electrode.
Burette
A graduated cylindrical piece of laboratory glassware that is used to dispense precise amounts of solution.
Complex Ion
A species where a central metal ion is covalently bonded to one or more electron donating groups called ligands.
Complexometric Titrations
Metal ions are titrated using a titrant that binds strongly to it. The titrants often contain Ethylenediaminetetraacetic Acid
(EDTA) or Cyclohexylenedinitrilotetraacetic Acid (CDTA).
End point
The point where a titration is stopped because a physical change in the solution has indicated a completed titration.
Titration end points typically coincide with the equivalence point. A fixed value end point (pH or mV) can be used as well.
The titration will stop at the desired point regardless of whether the titration is complete.
4-21
TITRATION THEORY
4
Equivalence point
The point where the quantity of titrant is stoichiometrically equal to the quantity of analyte.
Formal
The theoretical number of equivalents per liter of the solution. It is used in solutions where the exact concentration of a
species may be affected by the other ions present, therefore the stated concentration may not be exactly correct.
Gravimetric Analysis
A quantitative determination of an analyte based on the mass of the solid.
Indicator Electrode
An electrode that responds to the species of interest. The electrode potential is proportional to the concentration or
activity of that ion in the solution being measured.
Indicators
Chemical indicators are typically organic dyes that change form under different physical conditions, causing a color
change that can be seen by an analyst. Typically used in manual titrations. Chemical indicators have been replaced with
electrometric indicators, which are used with automatic titrators.
Inflection Point
The point on a titration curve were the second derivative curve changes signs.
Ion Selective Electrode (ISE)
An electrode that responds to a specific ion, the electrode potential is proportional to the concentration or activity of that
ion in the solution being measured.
Karl Fischer Titration
A titration that uses a chemical reaction that is specific for determining water.
Manual Titration
A titration that is carried out by hand, the analyst must add the appropriate amount of titrant, determine the end point
and calculate the results.
Molar
The concentration of a solute in a solution.
Mole (mol)
A quantity of a chemical species. The molecular weight of a substance in grams is equal to the mass of one mole of the
substance. One mole is equal to 6.022 x 1023 atoms or molecules.
Monochromator
A device that allows only a narrow range of wavelengths to pass though it by separating the light into different
wavelengths.
Multiple End Point Titration
A titration that reacts multiple species in solution, sequentially using the same titrant. The concentration of each analyte
can be determined from their respective end points.
Nernst Equation
The fundamental equation relating cell voltage to the concentration of a solution.
Neutralization
A chemical reaction where an acid and a base react to form a neutral salt and water.
4-22
Non-aqueous
A solution that does not contain water.
Normal
The concentration of a solution which accounts for any stoichiometric difference between the various species in a solution.
Oxidation/ Reduction Potential (ORP)
A voltage generated in a solution which is a result of the ratio of the oxidized to reduce species. Typically measured
potentiometrically with an ORP sensor.
TITRATION THEORY
Non-aqueous Titration
A titration that is preformed in non-aqueous solutions. Typically used to titrate very weak acid and bases to eliminate
the leveling effect water has on all acids and bases dissolved in it.
4
Oxidant
The species that is accepting electrons in a redox reaction.
Pipette
Scientific apparatus that is used to deliver precise volumes of liquids.
Polyprotic Acid
Acids that are capable of donating more than one proton per acid molecule.
Potentiometric Titration
A titration in which the end point is determined by monitoring the voltage of the solution using an electrode.
Precipitation Titration
A titration in which the analyte reacts with the titrant to form an insoluble compound. The end point is typically detected
with an ISE sensitive to either the analyte or titrant.
Reagent
The chemical added in a titration that causes the given reaction to occur.
Reduction-Oxidation Reaction (redox)
A chemical reaction in which the atoms involved in the reaction have their oxidation numbers changed. Reduction is the
gain of electrons, which decreases the oxidation number. Oxidation is the loss of electrons, which increases the oxidation
number.
Reductants
The electron donor in a redox reaction.
Reference Electrode
An electrode that supplies a constant electrode potential. It is used in combination with an “indicator” electrode,
allowing for the “indicator” electrode potential to be measured.
Relative Standard Deviation (RSD)
A measure of the amount of relative variation in a set of data. It is calculated by dividing the standard deviation by the mean:
RSD = (Standard Deviation of X) * 100 / (Mean of X)
Repeatability
The variation in sample measurements taken by a single person or instrument under the same conditions.
Spectrophotometric Titration
A titration in which the end point is marked by a change in the color and/or color intensity.
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TITRATION THEORY
4
Stoichiometry
The quantitative relationship of the reactants and products in a chemical reaction.
Titrant
The chemical added in a titration that causes the given reaction to occur.
Titration
A quantitative, volumetric procedure used in analytical chemistry to determine the concentration of an analyte in
solution. The concentration of the analyte is determined by slowly adding a titrant to the solution. As the titrant is
added, a chemical reaction between the titrant and the analyte occurs.
Titration Curve
A graph containing the physical data obtained for a titration. The data plotted is often an independent variable (volume
of titrant) vs. a dependent variable (pH of the solution). From the titration curve, the equivalence point or end point can
be determined.
MAN933
4-24
10/19
Certification
All Hanna Instruments conform to the CE European Directives.
Disposal of Electrical & Electronic Equipment. The product should not be treated as
household waste. Instead hand it over to the appropriate collection point for the recycling
of electrical and electronic equipment which will conserve natural resources.
Ensuring proper product and battery disposal prevents potential negative consequences
for the environment and human health. For more information, contact your city, your local
household waste disposal service, the place of purchase or go to www.hannainst.com.
Recommendations
for Users
Before using this product, make sure it is entirely suitable for your specific application and
for the environment in which it is used. Any variation introduced by the user to the supplied
equipment may degrade the meters’ performance. For yours and the meter’s safety do not
use or store the meter in hazardous environments.
Warranty
The HI933 is warranted for two years against defects in workmanship and materials when
used for its intended purpose and maintained according to instructions. Damage due to
accidents, misuse, tampering or lack of prescribed maintenance is not covered.
If service is required, contact your local Hanna Instruments Office. If under warranty, report
the model number, date of purchase, serial number and the nature of the problem. If
the repair is not covered by the warranty, you will be notified of the charges incurred.
If the instrument is to be returned to Hanna Instruments, first obtain a Returned Goods
Authorization (RGA) number from the Technical Service department and then send it with
shipping costs prepaid. When shipping any instrument, make sure it is properly packed for
complete protection.
Hanna Instruments reserves the right to modify the design, construction or appearance of its products
without advance notice.
World
Headquarters
Hanna Instruments Inc.
Highland Industrial Park
584 Park East Drive
Woonsocket, RI 02895 USA
www.hannainst.com
MAN933
Printed in ROMANIA
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