Hanna Instruments | HI931 | Owner Manual | Hanna Instruments HI931 Owner Manual

Hanna Instruments HI931 Owner Manual
AUTOMATIC
POTENTIOMETRIC TITRATOR
MANUALS
HI931
Congratulations on choosing your new Hanna titrator. It is a powerful and versatile instrument capable of accurate and fast
analysis of a wide range of samples. In this manual you’ll find:
QUICK START GUIDE
This guide will help you quickly setup, operate, and introduce you to your new titrator. It covers basic connections, user interface,
how to perform calibrations, and how to run a titration.
INSTRUCTION MANUAL
The manual provides a comprehensive description of the operating principles user interface, general options, methods, titration/
direct reading mode, pH, mV and ISE mode, maintenance, etc.
APPLICATIONS BROCHURE
This brochure contains complete instructions for commonly-used analyses. Additional methods and method packs are available;
contact your local Hanna office for more details.
TITRATION THEORY
This guide outlines the principles of operation of the titrator. It covers the chemistry of titrations, titration types, and result
calculations.
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.
TABLE OF CONTENTS
HI931 AUTOMATIC POTENTIOMETRIC TITRATOR
AUTOMATIC
POTENTIOMETRIC TITRATOR
QUICK START GUIDE
HI931
Dear
Customer,
Congratulations on choosing a Hanna Instruments product.
Please read this Quick Start Guide carefully before using the instrument. This guide will provide you with the necessary
information for the correct use of the instrument.
The purpose of this guide is to present a quick overview of setting up and using the instrument.
For detailed information illustrating the extensive capabilities of your titrator, please refer to the Instruction Manual.
© 2018 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.
QUICK START GUIDE
INTRODUCTION.................................................................................................................................................................. 4
SAFETY MEASURES............................................................................................................................................................ 4
TITRATOR CONNECTIONS.................................................................................................................................................. 5
USER INTERFACE................................................................................................................................................................ 6
HOW TO SELECT YOUR LANGUAGE................................................................................................................................... 7
HOW TO USE THE CONTEXTUAL HELP.............................................................................................................................. 7
METHODS........................................................................................................................................................................... 7
HOW TO CALIBRATE A pH ELECTRODE.............................................................................................................................. 7
HOW TO PERFORM A TITRATION....................................................................................................................................... 8
3
QUICK START GUIDE
INTRODUCTION
The HI931 automatic titrator is designed to perform a wide variety of potentiometric titrations with high accuracy, flexibility and
reproducibility, allowing the user to obtain both accurate results and high-speed analysis.
The titrator can perform fixed endpoint or equivalence point titrations and direct measurements by measuring the pH/mV and
temperature of the sample.
Reports and methods can be transferred to a PC via a USB interface, saved to a USB storage device or printed directly from the
titrator. An external keyboard can also be attached for added convenience.
How can I find certain information?
- The Quick Start Guide will help the user learn how to operate the titrator within a short period of time.
-The Instruction Manual provides a complete description of the operating principles (user interface, general options, methods,
titration, pH, mV and ISE mode, maintenance, etc.).
- The Titration Theory outlines the basic concepts of titration.
- The contextual Help screens contain detailed explanations of every screen.
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 bottle and the titration beaker are placed on a flat, stable surface.
4. Always wipe up spills and splashes immediately.
5. Avoid the following environmental working conditions:
• Severe vibrations
• Direct sunlight
• Atmospheric relative humidity above 95% non-condensing
• Environment temperatures below 10°C and above 40°C
• Explosion hazards
6. Have the titrator serviced by qualified service personnel only.
4
FRONT VIEW
QUICK START GUIDE
TITRATOR CONNECTIONS
REAR VIEW
5
QUICK START GUIDE
USER INTERFACE
Keypad
The titrator’s keypad has 27 keys grouped in five categories, as follows:
Display
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 option key is pressed.
6
To change the language, press
from the main screen. Highlight the Language option. Using the
the language and press
.
Restart the titrator in order to apply the new language setting.
and
keys, select
QUICK START GUIDE
HOW TO SELECT YOUR LANGUAGE
HOW TO USE THE CONTEXTUAL HELP
Information about the titrator can be easily accessed by pressing
provides useful information about the current screen.
. The contextual help can be accessed at any time and it
METHODS
The HI931 titrator can store up to 100 methods (standard and user).
Standard Methods
Each titrator is supplied with a package of standard methods. Standard method packs are developed at Hanna Instruments to meet
analysis requirements of specific industries (e.g., water treatment, wine, dairy, etc.).
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.
HOW TO CALIBRATE A pH ELECTRODE
To enter pH calibration mode, press
, then
, then
.
PREPARATION
Pour small quantities pH 4.01, pH 7.01 and pH 10.01 buffer solutions into clean beakers. If possible, use plastic beakers to
minimize any EMC interferences.
For accurate calibration and to minimize cross-contamination, use two beakers for each buffer solution: one for rinsing the electrode
and one for calibration.
CALIBRATION PROCEDURE
• If the instrument has been previously calibrated and calibration was not cleared, the old calibration can be cleared by pressing
.
Note: It is very important to clear calibration history when a new electrode is used. Most errors and warning messages that appear
during calibration depend on calibration history.
7
QUICK START GUIDE
• Use the
or
to select pH 4.01 buffer solution.
• Use the second beaker of pH 4.01 buffer solution to rinse the pH electrode, temperature probe and propeller stirrer.
•Immerse the pH electrode, temperature probe and propeller stirrer in the pH 4.01 buffer solution. The pH electrode’s bulb must
be completely immersed in the buffer solution and the reference junction needs to be 5-6 mm below the surface. Add additional
buffer if necessary.
• Press
to turn on the propeller stirrer.
• Once the reading has stabilized, press
to update the calibration.
• Repeat this procedure for pH 7.01 and 10.01 buffer solutions.
• Press
to accept and exit pH calibration mode.
HOW TO PERFORM A TITRATION
Required Solutions
• Titrant - 500 mL of 0.1 M (mol/L) Sodium Hydroxide (NaOH) in a titrant bottle.
• Sample - 0.1 mol/L Hydrochloric Acid (HCl).
• Distilled or deionized water.
Note: Analytical grade reagents and water should be used for accurate results.
Priming the Burette
• Insert the aspiration tube in the titrant bottle and the dispensing tube in a waste beaker.
• From the main screen press
.
•Highlight the Prime Burette option and then press
.
•Enter the number of burette rinses. At least 3 rinses are recommended.
•Press
to start.
•The message “Executing...” will be displayed.
Note: Make sure you have continuous liquid flow inside the burette. For accurate results, the aspiration tube, the dispensing tube
and the syringe must be free of air bubbles.
Method Selection
For this analysis, we will use the HI1009 Neutralization w/ NaOH.
To select this method:
• Press
. Use the
and
keys to highlight HI1009 Neutralization w/ NaOH.
• Press
.
Setting Method Parameters
To display the method parameters, press
.
The View/Modify Method screen will be displayed.
Only certain parameters can be changed.
For this titration, the NaOH titrant concentration and the size of the HCl sample need to be entered.
To accomplish this:
• Highlight Titrant Conc. option, then press
.
The Titrant Concentration screen will be displayed.
• Enter the correct value, then press
.
• Highlight Analyte Size option, then press
.
• Enter the volume of the sample (e.g.: 5 mL), then press
.
• Press
, highlight Save Method option and then press
.
8
QUICK START GUIDE
Setup Titration Report
Users can select the information that is stored for each titration.
To setup the titration report, follow the procedure below:
• From the main screen, press
. The Data Parameters screen will be displayed.
• Highlight Setup Titration Report and press
.
•Mark the fields to be included in the titration report with the “*” symbol. Use the
and
/
to toggle the field.
keys to highlight a field and
• Press
to save the customized report .
Preparing the Sample
• Add 50 to 65 mL of distilled/deionized water to the titration beaker.
• Use a pipette or burette to add 5.0 mL of the sample (0.1M Hydrochloric Acid (HCl)) into the same beaker.
• Slide the stirrer assembly up.
• Place the beaker under the stirrer assembly.
• Lower the stirrer assembly until the electrodes are submersed and the stirrer is close to the bottom of the beaker.
•Adjust the level of the sample solution with distilled/deionized water so that the pH electrode bulb is completely immersed in
the sample solution and the reference junction of the electrode is 5-6 mm below the surface.
Performing a Titration
•From the main screen, press
. You will be prompted to enter the analyte size. Enter 5 mL and press
. The titrator will
start the analysis.
•At the end of the titration, the message “Titration Completed” will appear on the display with the final concentration of the
analyte in the sample and the equivalence endpoint volume.
Understanding the Displayed Information
During a titration the following screen is displayed:
9
QUICK START GUIDE
Viewing Graph During Titration
After a few doses are dispensed,
will become active. Press
to display the real-time titration graph.
The curves displayed are plots of the pH and the 1st derivative versus Titrant Volume (for details, see the Instruction Manual).
The two graphs are scaled to fit in the same screen window. Press
to change the y-axis scale to either the pH values or the
1st derivative values.
Titration Termination
The titration is normally terminated when the first equivalence endpoint is detected according to the selected algorithm. To ensure the
correct detection and interpolation of the equivalence endpoint, the titrator will dispense a few additional doses after the endpoint
was reached.
The titration result can be displayed either in the main screen or in the Graph of Titration Data screen:
10
QUICK START GUIDE
When the titration has ended, the titrator will display the equivalence endpoint volume and the final concentration of the analyte
together with the "Titration Completed" message.
To view the titration graph and/or results, press
.
When the titration ends, an “x” will mark the endpoint on the pH versus titrant volume curve in the Graph of Titration Data
screen. The value of the endpoint volume is also displayed next to the endpoint.
Results
The results obtained from a titration are stored in a report file that can be viewed, transferred to a USB Storage Device or PC and
printed.
Viewing the last titration data
• From the main screen, press
. The Data Parameters screen will be displayed.
• From the Data Parameters screen highlight the Review Last Analysis 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.
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: When connecting the printer, please turn off the titrator and the printer.
Printing out the report:
• From the Review Report screen, press
.
• During the information transfer to the printer, the message “Printing” will be displayed on the screen.
• Press
to return to the Data Parameters screen.
• Press
again to return to the main screen.
Saving data to USB Storage Device
This feature allows saving the results of titrations or pH / mV / ISE logging sessions on a USB storage device.
•From the main screen, press
, the General Options screen will be displayed.
•Highlight the 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.
11
QUICK START GUIDE
• 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.
Titration report
While scrolling with the
and
keys, the fields below can be seen on the titrator display or printed. The same
information is available on the saved report file (Ti_00007.rpt in this example).
HI931 - Titration Report
Method Name:
Time & Date:
Report ID:
Neutralization w/ NaOH
15:01 Jun 13, 2018
Ti_00011
Calibration Data
Buffer
Potential
Efficiency Temp.
Time and Date
4.010pH 169.3mV 98.8% 24.0°C A
11:44 Jun 13, 2018
7.010pH -5.8mV 98.7% 23.9°C A
11:42 Jun 13, 2018
10.010pH -180.7mV 98.7% 24.0°C A
11:46 Jun 13, 2018 GLP & Meter Information
Sample Name:
Company Name: Operator Name:
Electrode Name: Field 1:
Field 2:
Field 3:
Titrator Software Version: v1.00
Base Board Software Version: v1.00
Pump 1 Software Version: v1.00
Stirrer 1 Software Version: v1.00
Titrator Serial Number:
TT180525011
Analog Board1 Serial Number:AB180525005
Pump 1 Serial Number: DP180525004
Stirrer 1 Serial Number:
OS180524001
Analog 1 Calibration Date: May 25, 2018
Method Parameters
Name:
Neutralization w/ NaOH
Method Revision: 3.0
Analysis Type: Standard Titration
Stirrer Configuration:
Stirrer:
Stirrer 1
Stirring Speed: 1400 RPM
12
QUICK START GUIDE
Pump Configuration:
Titrant pump: Pump 1
Dosing Type: Dynamic
Min Vol: 0.050 mL
Max Vol: 0.500 mL
delta E: 20.000 mV
End Point Mode: pH 1EQ point,1st Der
Recognition Options
Threshold: 50 mV/mL
Range: NO
Filtered Derivatives: NO
Pre-Titration Volume: 0.000 mL
Pre-Titration Stir Time: 0 sec
Measurement Mode: Signal Stability
delta E: 1.0 mV
delta t: 2 sec
Min wait: 2 sec
Max wait: 15 sec
Electrode Type: pH
Blank Option:
No Blank
Calculations: Sample Calc. by Volume
Dilution Option: Disabled
Titrant Name: 0.1N HaOH
Titrant Conc.: 0.1000 N (eq/L)
Analyte Size: 10.0000 mL
Analyte Entry: Fixed
Maximum Titrant Volume: 20.000 mL
Potential Range: -2000.0 to 2000.0 mV
Volume/Flow Rate: 25 mL / 50.0 mL/min
Signal Averaging: 1 Reading
Significant Figures: XXXXX
N (eq/L) --> meq/L
V eq 1000meq
-*--*------ L eq ------------mL
L
--*-----1000mL
V = volume dispensed in liters.
0.100 eq/L -> titrant conc.
10.000 mL -> sample volume
Nr Volume[mL] mV pH Graphic Temp.[°C] Time
0 0.000 274.4 2.219 0.0 24.9 A 00:00:00
1 0.050 274.4 2.220 1.0 25.0 A 00:00:07
2 0.100 274.4 2.220 0.0 25.0 A 00:00:10
3 0.200 274.3 2.222 -0.8 25.0 A 00:00:12
4 0.400 274.0 2.227 -1.6 25.0 A 00:00:15
5 0.800 273.2 2.241 -2.0 25.0 A 00:00:18
6 1.300 271.5 2.271 -3.4 25.0 A 00:00:24
7 1.800 269.5 2.304 -3.9 25.1 A 00:00:30
8 2.300 267.2 2.344 -4.7 25.1 A 00:00:37
9 2.800 264.4 2.393 -5.7 25.1 A 00:00:43
10 3.300 260.8 2.455 -7.2 25.1 A 00:00:50
11 3.800 256.1 2.535 -9.3 25.1 A 00:00:58
12 4.300 250.3 2.635 -11.7 25.1 A 00:01:05
13 4.800 241.9 2.779 -16.8 25.1 A 00:01:14
14 5.300 228.3 3.011 -27.2 25.1 A 00:01:23
13
QUICK START GUIDE
15 5.800 193.0 3.614 -70.5 25.1 A
16 6.077 21.0 6.556 -620.0 25.1 A
17 6.128 -38.2 7.568 -1183.2 25.1 A
18 6.177 -123.6 9.031 -1708.0 25.1 A
19 6.227 -157.7 9.616 -682.8 25.1 A
20 6.278 -174.5 9.903 -335.8 25.1 A
21 6.339 -187.8 10.130 -215.9 25.1 A
00:01:31
00:01:48
00:02:03
00:02:19
00:02:28
00:02:35
00:02:42
Titration Results
Method Name:
Neutralization w/ NaOH
Time & Date:
15:01 Jun 13, 2018
Analyte Size: 10.0000 mL
End Point Volume: 6.144 mL
pH Equivalence Point: 8.063
Result: 61.444 meq/L
Initial & Final pH: 2.219 to 10.130
Titration Duration: 2:42 [mm:ss]
Titration went to Completion
Analyst Signature: ____________________
QS931 10/18
14
AUTOMATIC
POTENTIOMETRIC TITRATOR
INSTRUCTION MANUAL
HI931
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.
© 2018 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.
TABLE OF CONTENTS
CHAPTER 1. INTRODUCTION
CHAPTER 2. SETUP
CHAPTER 3. USER INTERFACE
CHAPTER 4. GENERAL OPTIONS
CHAPTER 5. TITRATION METHODS
CHAPTER 6. TITRATION MODE
CHAPTER 7. pH MODE
CHAPTER 8. mV MODE
CHAPTER 9. ISE MODE
CHAPTER 10. AUXILIARY FUNCTIONS
CHAPTER 11. MAINTENANCE, PERIPHERALS
APPENDIX 1. TECHNICAL SPECIFICATIONS
APPENDIX 2. ACCESSORIES
CERTIFICATION
RECOMMENDATIONS FOR USERS
WARRANTY
• Small footprint, requires minimal bench space
INTRODUCTION
1. INTRODUCTION
HI931 is an automatic potentiometric titrator with high accuracy, great flexibility and repeatability.
The titrator is designed to perform a variety of potentiometric titrations, allowing the user to obtain both good results and high-speed
analysis.
The main attributes of the HI931 titrator are:
• Casing made with strong, chemically resistant plastic
• Flexible electrode holder supports up to 3 electrodes, 4 dispensing tubes, 1 temperature sensor and removable stirrer
• Electrode holder positions electrodes in the center of beaker, allowing for smaller sample sizes
• Integrated Peristaltic Pump available for reagent addition
• Support for 100 titration methods
• User-customizable reports
• Integrated research grade pH/mV/ISE meter
• 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.
1-1
1-2
2.1. UNPACKING................................................................................................................................................................2-3
2.2. SAFETY MEASURES.....................................................................................................................................................2-4
2.3. INSTALLATION............................................................................................................................................................2-4
2.3.1. TITRATOR FRONT VIEW...............................................................................................................................................2-4
2.3.2. TITRATOR REAR VIEW.................................................................................................................................................2-5
2.3.3. TITRATOR REAR VIEW WITH PERISTALTIC PUMP............................................................................................................2-5
2.3.4. TITRATOR RIGHT-SIDE VIEW........................................................................................................................................2-6
2.3.5. TITRATOR ASSEMBLY..................................................................................................................................................2-6
2.3.5.1. ASSEMBLING STIRRER AND ELECTRODES HOLDER................................................................................................2-6
2.3.5.2. ATTACHING STIRRER AND ELECTRODES................................................................................................................ 2-7
2.3.5.3. CONNECTING THE PUMP.....................................................................................................................................2-8
2.3.5.4. ATTACHING BURETTE BLANK SUPPORT................................................................................................................ 2-8
2.3.5.5. ATTACHING THE BURETTE...................................................................................................................................2-9
2.3.5.6. CONNECTING PERISTALTIC PUMP TUBING............................................................................................................2-10
2.3.5.7. ELECTRICAL CONNECTIONS..................................................................................................................................2-11
SETUP
CHAPTER 2. SETUP
2-1
2-2
ITEM
SETUP
2.1. UNPACKING
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 HI931 potentiometric titrator is supplied with:
QUANTITY
Titrator............................................................................................................................................................................... 1 pc
Pump Assembly................................................................................................................................................................... 1 pc
Burette Assembly................................................................................................................................................................. 1 pc
• Burette (with 25-mL syringe)
• Aspiration Tube with Fitting and Protection Tube
• Dispensing Tube with Normal Dispensing Tip, Fitting, Protection Tube and Tube Guide
• Tube Locks
• Tool for Burette Cap Removal
• Light Spectrum Protection Screen
Electrodes Holder and Stirrer................................................................................................................................................ 1 pc
• Stirrer Holder
• Overhead Stirrer
• Propellers (3 pcs)
• Support Rod
Burette Blank Support.......................................................................................................................................................... 1 pc
Pump and Burette Locking Screws with Plastic Head..............................................................................................................2 pcs
Temperature Sensor............................................................................................................................................................. 1 pc
Shorting Cap....................................................................................................................................................................... 1 pc
Power Adapter..................................................................................................................................................................... 1 pc
USB Cable.......................................................................................................................................................................... 1 pc
Instruction Manual.............................................................................................................................................................. 1 pc
USB Memory Stick............................................................................................................................................................... 1 pc
HI900 PC Application (Installation Kit on USB Stick).............................................................................................................. 1 pc
Quality Certificate................................................................................................................................................................ 1 pc
See APPENDIX 2, titrator components 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.
2-3
SETUP
2.2. SAFETY MEASURES
The following safety measures must be followed:
1. Never connect or disconnect the pump assembly 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 bottle and the titration beaker are on a flat surface.
4. Always wipe up spills and splashes immediately.
5. Avoid the following environmental working conditions:
• Severe vibrations
• Direct sunlight
• Atmospheric relative humidity above 95% 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. INSTALLATION
2.3.1. TITRATOR FRONT VIEW
2-4
SETUP
2.3.2. TITRATOR REAR VIEW
2.3.3. TITRATOR REAR VIEW WITH PERISTALTIC PUMP
2-5
SETUP
2.3.4. TITRATOR RIGHT-SIDE VIEW
2.3.5. TITRATOR ASSEMBLY
Note: Assembly operations must be completed before connecting the Titrator to the power supply!
2.3.5.1. ASSEMBLING STIRRER AND ELECTRODES HOLDER
To assemble the electrode holder and support rod:
• Remove protective cap from titrator case
• Insert the support rod into the titrator case and turn it clock-wise to secure it in place
2-6
SETUP
2.3.5.2. ATTACHING STIRRER AND ELECTRODES
To attach the stirrer to the titrator, follow these steps:
• Place the electrodes holder (B) in the stirrer support housing (A). Stirrer support housing can be inverted if necessary.
• Insert electrode (C), temperature sensor (D) and stirrer (E) into the dedicated holes in the electrode holder. Push them until
they are in stable position.
Note: For small sample sizes, use the electrode adapter (F) in the center of the holder.
• Slide the electrode holder into the support rod and set the desired height using the holder button.
2-7
SETUP
2.3.5.3. CONNECTING THE PUMP
To connect the pump, follow these steps:
• Retrieve the pump cable from inside the bay. The pump 1 connector is located in the left bay and pump 2 in the right bay.
• Connect the cable to the pump as shown below. The pump connector is located on the bottom of the pump.
• Lower the pump into the titrator, then slide it towards the front of the titrator case until it is firmly latched.
• Secure the pump with the locking screw.
This procedure can be repeated to connect a second pump.
2.3.5.4. ATTACHING BURETTE BLANK SUPPORT
To attach the burette blank support, follow these steps:
• Insert burette blank support into the bay. Lower the burette blank support into the titrator, then slide it towards the front of
the titrator case until it is firmly latched.
• Secure the burette blank support with the locking screw.
2-8
SETUP
2.3.5.5. ATTACHING THE BURETTE
Make sure that the mark from the valve actuating cap and from the burette body are aligned.
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.
2-9
SETUP
2-10
2.3.5.6. CONNECTING PERISTALTIC PUMP TUBING
To attach the pump tubing to the burette pump with the built-in peristaltic pump:
• Use a screw driver to remove the plastic cover (E) from the pump.
• Remove the blue tube connectors (F).
• Insert the roller tube (C) into the left side of the holder (D). The fitting on the top of the roller tube will sit in the top of the
housing.
• Manually rotate the pump (A) counter-clock wise until the tubing it mounted on the pump.
• Insert the roller tube (B) into the right side of the holder (G). The fitting on the top of the roller tube will sit in the top of the
housing.
• Attach aspiration and dispensing tubing to the roller tubing and replace the blue tube connectors (F).
• Replace the plastic cover (E).
Nr Function
Connection for pH, ORP, ISE half-cell and
A
ISE combination electrodes
B Reference electrode
C Temperature sensor
D Stirrer
E USB interface
F Power input connector (24VDC)
G External PC keyboard
H Printer
I Extension interface
J RS232 interface (Balance Interface)
K Power switch
SETUP
2.3.5.7. ELECTRICAL CONNECTIONS
• Connect the electrode to the BNC connector (A).
• Connect the temperature sensor to the RCA connector (C).
• Connect the stirrer to the MINI-DIN connector (D).
• Connect the power adapter cable to the power input connector (F).
Type of Connector
BNC Socket
4 mm Banana Socket
RCA Socket
6-pin Connector
USB Standard B
DC Power Jack Connector
6-pin Mini DIN (Standard PS2)
DB-25 Socket
5-pin Connector
DB-9 Socket
2-11
2-12
3.1. START UP...................................................................................................................................................................3-3
3.2. DESCRIPTION.............................................................................................................................................................3-4
3.2.1. KEYPAD.....................................................................................................................................................................3-4
3.2.1.1. FUNCTION KEYS.................................................................................................................................................3-4
3.2.1.2. OPTION KEYS....................................................................................................................................................3-4
3.2.1.3. ARROW KEYS.....................................................................................................................................................3-5
3.2.1.4. NUMERIC KEYS..................................................................................................................................................3-5
3.2.1.5. ENTER KEY........................................................................................................................................................3-5
3.2.2. DISPLAY....................................................................................................................................................................3-5
3.2.3. THE MAIN SCREEN.....................................................................................................................................................3-6
3.3. MENU NAVIGATION....................................................................................................................................................3-7
3.3.1. SELECTING AN OPTION................................................................................................................................................3-7
3.3.2. SELECTING A MENU ITEM............................................................................................................................................3-7
3.3.3. ENTERING TEXT..........................................................................................................................................................3-7
3.3.4. SAVING MODIFICATIONS.............................................................................................................................................3-8
USER INTERFACE
CHAPTER 3. USER INTERFACE
3-1
3-2
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
USER INTERFACE
3.1. START UP
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 Service Center.
3-3
USER INTERFACE
3.2. DESCRIPTION
This chapter describes the basic principles of navigating through the user interface, selecting fields and entering values from the
keypad.
3.2.1. KEYPAD
The titrator’s keypad is grouped into five categories, as follows:
3.2.1.1. 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
Turns the selected stirrer On and Off
Reserved
Access the Data Parameters Menu (reports, GLP, meter information, report setup)
Displays Contextual Help
3.2.1.2. 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
.
3-4
USER INTERFACE
3.2.1.3. ARROW KEYS
These keys have the following functions:
• Move the on-screen cursor.
• Increase and decrease the stirrer speed and other settings.
• In the alphanumeric screen, to select a character.
• Navigate through menu options.
3.2.1.4. NUMERIC KEYS
Keys
to
Used for numeric entries.
Toggles between positive and negative values.
Decimal point.
3.2.1.5. ENTER KEY
This key has the following functions:
• Accept alphanumeric data entry.
• Executes the default (underlined) virtual option key.
3.2.2. DISPLAY
The titrator has a large color graphical display. The main screen is shown below with short explanations of the screen segments.
3-5
USER INTERFACE
The user interface contains several screens. For each titrator function, one or more screens are used.
3.2.3. THE MAIN SCREEN
After start up and initialization, the first screen displayed is the main screen.
Main screen fields:
Method name:
Time and date:
Temperature reading:
ATC:
Manual:
Manual :
Stirrer information:
End point volume:
Result:
mV or pH reading:
mV:
rel mV:
pH:
Titration status:
Displays the name of the selected method.
Displays the current date and time.
Displays the measured temperature.
Automatic temperature compensation
Manual temperature compensation
Temperature probe is not connected, manual temperature compensation
The selected stirrer and actual/set stirrer speed is displayed in RPM. When stirrer is off,
the stirrer information is not displayed.
Displays the volume delivered to reach the titration end point. When no titration
has been performed, the displayed volume is “0.000 mL”.
Displays the titration result or the direct reading measurement.
Displays the current readings. The reading will be in mV or pH.
Indicates actual potential reading.
Indicates relative potential reading.
Indicates actual pH value.
Displays the status of the selected titration.
No Results is displayed when a titration has not been performed.
Reminders: Indicates when a task needs to be performed and displays error
Pump 1 selected: Displays the active pump.
3-6
USER INTERFACE
3.3. MENU NAVIGATION
3.3.1. SELECTING AN OPTION
To select an option, simply press the option key below the virtual key. For example, to
access the Method Options screen press the option key below it.
3.3.2. SELECTING A MENU ITEM
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.
The
and
keys can be used to scroll through the pages.
To activate the selected menu item, press
or
.
3.3.3. ENTERING TEXT
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
.
3-7
USER INTERFACE
3.3.4. SAVING MODIFICATIONS
The Saving Method screen allows the user to save the modifications. To exit from
Saving Method screen without saving, press
or highlight the Exit Without
Saving Method option and then press
. To save the modifications highlight the
Save Method option and then press
.
Note: T o access the contextual help menu, press
to return to the previous screen.
3-8
at any time. Help is related to the displayed screen. Press
or
4.1. SAVE FILES TO USB STORAGE DEVICE.......................................................................................................................4-3
4.2. RESTORE FILES FROM USB STORAGE DEVICE...........................................................................................................4-4
4.3. ADMINISTRATION......................................................................................................................................................4-5
4.4. TEMPERATURE...........................................................................................................................................................4-6
4.4.1. TEMPERATURE SOURCE..............................................................................................................................................4-7
4.4.2. MANUAL TEMPERATURE SETTING.................................................................................................................................4-7
4.4.3. TEMPERATURE UNITS.................................................................................................................................................4-8
4.5. DATE AND TIME SETTING...........................................................................................................................................4-8
4.6. DISPLAY SETTINGS....................................................................................................................................................4-8
4.7. BEEPER.......................................................................................................................................................................4-9
4.8. STIRRER......................................................................................................................................................................4-10
4.9. LANGUAGE.................................................................................................................................................................4-10
4.10. TOTAL VOLUME ALERT.............................................................................................................................................4-10
4.11. TITRANT AGE REMINDER.........................................................................................................................................4-11
4.12. USB LINK WITH PC...................................................................................................................................................4-11
4.13. SETUP BALANCE INTERFACE....................................................................................................................................4-12
4.14. PRINTER MODE........................................................................................................................................................4-13
4.15. RESET TO DEFAULT SETTINGS.................................................................................................................................4-13
4.16. OPTIMIZE MEMORY SPACE.......................................................................................................................................4-14
4.17. UPDATE SOFTWARE.................................................................................................................................................4-14
GENERAL OPTIONS
CHAPTER 4. GENERAL OPTIONS
4-1
4-2
GENERAL OPTIONS
The General Options screen gives access to options that are not directly related to the titration process or pH/mV/ISE measurement.
To access this screen, press
from the main screen.
4.1. SAVE FILES TO USB STORAGE DEVICE
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.: HI0001EN.MTD, HI1004EN.MTD)
User Method Files
-USERXXXX.MTD (e.g.: USER0001.MTD)
Report Files
-Ti_XXXXX.RPT, mV_XXXXX.RPT, pH_XXXXX.RPT, ISEXXXXX.RPT, mVrXXXXX.RPT
(e.g.: Ti_00001.RPT, mV_00001.RPT, pH_00001.RPT, ISE00001.RPT, mVr00001.RPT)
Use the
and
keys to select the file type. The number of files and the file name on the titrator will be displayed.
4-3
GENERAL OPTIONS
The option keys allow the following operations:
Deletes the highlighted file.
Deletes all currently displayed files.
Copies the highlighted file from titrator to a USB storage device.
Copies all currently displayed files from titrator to a USB storage device.
Returns to the General Options screen.
The status of the transfer (“Successful”/“Unsuccessful”) and the file name of the currently processed file are displayed during copying or
deleting.
Note: The saved files will be stored on the USB key in the HI931 folder, as follows:
- Methods: USB Drive:\HI931\Methods\*.mtd
- Reports: USB Drive:\HI931\Reports\*.rpt
4.2. RESTORE FILES FROM USB STORAGE DEVICE
This screen allows the user to transfer files from the USB storage device to the titrator.
Standard Method Files -HIXXXXYY.MTD (e.g.: HI0001EN.MTD, HI1004EN.MTD)
User Method Files
-USERXXXX.MTD (e.g.: USER0001.MTD)
Report Files
-Ti_XXXXX.RPT, mV_XXXXX.RPT, pH_XXXXX.RPT, ISEXXXXX.RPT, mVrXXXXX.RPT (e.g.: Ti_00001.
RPT, mV_00001.RPT, pH_00001.RPT, ISE00001.RPT, mVr00001.RPT)
Use the
and
keys to select the file type.
The number of files and the file name will be displayed.
4-4
Deletes the highlighted file from the USB storage device.
Deletes all currently displayed files from the USB storage device.
Copies the highlighted file from the USB storage device to the titrator.
Copies all currently displayed files from the USB storage device to the titrator.
GENERAL OPTIONS
The option keys allow the following operations:
Returns to the General Options screen.
Note: In order to restore files from a 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:\HI931\Methods\*.mtd
- Reports: USB Drive:\HI931\Reports\*.rpt
4.3. ADMINISTRATION
A 4-digit numeric PIN can be set to prevent unauthorized changes from being made.
When the user enters administration and a pin has not been set, the user will be prompted to enter a new PIN.
Once a PIN has been set, the titrator can be locked. When a titrator is locked, the users cannot modify methods or delete reports.
Basic functions are still available (review reports, save to USB, etc.).
4-5
GENERAL OPTIONS
To return to administrator mode, the titrator can be unlocked by entering the PIN.
If the PIN is lost or forgotten, press recovery pin and contact technical support to supply the required information.
4.4. TEMPERATURE
The Temperature Menu allows access to all of the settings related to temperature.
4-6
Option: Automatic Temperature or Manual Temperature
Select the temperature source used for temperature compensation.
When Automatic Temperature Compensation is selected, “ATC” is displayed on the main screen and the temperature is read by the
temperature probe.
When Manual Temperature is selected, “Manual” is displayed on the main screen and a preset temperature value is used for
temperature compensation.
Note: The selected temperature source will be indicated in the report files: A for Automatic and M for Manual.
GENERAL OPTIONS
4.4.1. TEMPERATURE SOURCE
4.4.2. MANUAL TEMPERATURE SETTING
Option: -5.0 to 105.0 °C (23.0 to 221.0 °F, 268.2 to 378.2 K)
If the temperature probe is not connected, the user can manually set the temperature used by the titrator for compensation.
4-7
GENERAL OPTIONS
4.4.3. TEMPERATURE UNITS
Option: °C, °F or K
The temperature ranges are as displayed in the Temperature Units screen.
4.5. DATE AND TIME SETTING
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.
4.6. DISPLAY SETTINGS
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
and
There are 8 levels of backlight intensity, ranging from 0 to 7.
4-8
keys.
GENERAL OPTIONS
A color palette is displayed in the center of the screen allowing an easy selection of the 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 display backlight is off, any keystroke will activate the backlight without performing any action.
The range for the backlight saver timer is 1 to 60 minutes. To disable the backlight saver, increase the time to the maximum allowed.
The “Off” indication will appear.
4.7. 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.
4-9
GENERAL OPTIONS
4.8. STIRRER
Option: Enabled or Disabled
The stirrer can be disabled in individual titration method, if necessary.
4.9. LANGUAGE
Option: English, Português, or Español
4.10. TOTAL VOLUME ALERT
Option: Off, 0 to 10000 mL
This screen allows a programmable reminder to appear when the titrant reservoir is below 100 mL. The titrant volume will decrease
as the titrant is used.
After the new titrant volume has been entered in the Total Volume Alert screen, a warning message appears on the main screen
reminding the user re-standardize the titrant.
4-10
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.
GENERAL OPTIONS
4.11. TITRANT AGE REMINDER
4.12. USB LINK WITH PC
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 information about the percentage of current file
already transferred are displayed.
4-11
GENERAL OPTIONS
4.13. SETUP BALANCE INTERFACE
This screen allows the users to connect an analytical balance for automatic acquisition of sample mass prior to titration or
standardization.
The balance is connected to the titrator via RS 232 interface.
Press
to add a new balance to the list.
Press
to enable the selected balance.
Press
to disable the selected balance (automatic weight acquisition will be not available).
Press
to customize the name and serial communication parameters used by the selected balance.
Be sure that the settings on the titrator Balance Configuration menu match the settings for your particular balance (baud rate, data
bits, parity, stop bits 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
4-12
key.
Option: Ansi, Ascii, or Text
GENERAL OPTIONS
4.14. PRINTER MODE
Ansi mode: U se this mode when your printer is set as Ansi. In this case all the accented characters/symbols available in titrator will
be printed on your printer.
Ascii mode: U se this mode when your printer is set as Ascii. In this case only some of the accented characters/symbols available in
titrator will be printed on your printer.
Text mode: Use this mode when you don’t need to print the accented characters.
4.15. RESET TO DEFAULT SETTINGS
Note: T his will also delete all the user - created methods and restore all manufacturer settings such as titrator configuration,
standard method parameters, etc.
4-13
GENERAL OPTIONS
4.16. OPTIMIZE MEMORY SPACE
4.17. UPDATE SOFTWARE
This screen allows the user to update the titrator software from a USB storage device containing a software setup kit.
To update the software:
• Copy the “Setup931” 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
4-14
. When prompted, remove the USB storage and restart the titrator.
TITRATION METHODS
CHAPTER 5. TITRATION METHODS
5.1. SELECTING METHODS................................................................................................................................................5-3
5.2. STANDARD METHODS................................................................................................................................................5-3
5.2.1. UPGRADING STANDARD METHODS...............................................................................................................................5-4
5.2.2. DELETING STANDARD METHODS..................................................................................................................................5-4
5.2.3. RESTORE THE STANDARD METHODS TO THE MANUFACTURER SETTINGS.........................................................................5-4
5.3. USER METHODS.........................................................................................................................................................5-5
5.3.1. CREATING USER METHODS..........................................................................................................................................5-5
5.3.2. DELETING USER METHODS..........................................................................................................................................5-5
5.4. VIEW / MODIFY METHOD...........................................................................................................................................5-6
5.5. METHOD OPTIONS.....................................................................................................................................................5-6
5.5.1. NAME........................................................................................................................................................................5-6
5.5.2. METHOD REVISION.....................................................................................................................................................5-7
5.5.3. STIRRER CONFIGURATION...........................................................................................................................................5-7
5.5.3.1. STIRRER............................................................................................................................................................5-7
5.5.3.2. STIRRER SPEED.................................................................................................................................................5-8
5.5.4. PUMP CONFIGURATION...............................................................................................................................................5-8
5.5.5. DOSING TYPE.............................................................................................................................................................5-9
5.5.5.1. LINEAR DOSING.................................................................................................................................................5-9
5.5.5.2. DYNAMIC DOSING..............................................................................................................................................5-10
5.5.6. END POINT MODE.......................................................................................................................................................5-11
5.5.6.1. FIXED END POINT (pH OR mV)............................................................................................................................5-11
5.5.6.2. EQUIVALENCE END POINT (pH OR mV)................................................................................................................5-12
5.5.7. RECOGNITION OPTIONS (EQUIVALENCE END POINT ONLY).............................................................................................5-15
5.5.7.1. THRESHOLD......................................................................................................................................................5-15
5.5.7.2. RANGE..............................................................................................................................................................5-16
5.5.7.3. FILTERED DERIVATIVES......................................................................................................................................5-17
5.5.12. PRE-TITRATION VOLUME...........................................................................................................................................5-18
5.5.13. PRE-TITRATION STIR TIME.........................................................................................................................................5-18
5.5.10. MEASUREMENT MODE..............................................................................................................................................5-19
5.5.10.1 SIGNAL STABILITY.............................................................................................................................................5-19
5.5.10.2 TIMED INCREMENT...........................................................................................................................................5-20
5.5.11. ELECTRODE TYPE......................................................................................................................................................5-21
5.5.12. BLANK OPTION.........................................................................................................................................................5-21
5.5.13. CALCULATIONS.........................................................................................................................................................5-22
5.5.13.1. STANDARD TITRATION......................................................................................................................................5-22
5.5.13.1.1. EDIT VARIABLE VALUES..............................................................................................................................5-22
5.5.13.1.2. NO FORMULA (mL ONLY)...........................................................................................................................5-22
5.5.13.1.3. NO FORMULA (L ONLY)..............................................................................................................................5-22
5.5.13.1.4. SAMPLE CALCULATION BY WEIGHT..............................................................................................................5-23
5-1
TITRATION METHODS
5-2
5.5.13.1.5. SAMPLE CALCULATION BY VOLUME.............................................................................................................5-24
5.5.13.1.6. STANDARDIZE TITRANT BY WEIGHT.............................................................................................................5-25
5.5.13.1.7. STANDARDIZE TITRANT BY VOLUME............................................................................................................5-26
5.5.13.1.8. GENERIC FORMULA....................................................................................................................................5-27
5.5.14. DILUTION OPTION....................................................................................................................................................5-29
5.5.15. TITRANT NAME.........................................................................................................................................................5-29
5.5.16. TITRANT CONCENTRATION.........................................................................................................................................5-30
5.5.17. ANALYTE SIZE...........................................................................................................................................................5-30
5.5.18. ANALYTE ENTRY........................................................................................................................................................5-30
5.5.18.1. FIXED WEIGHT OR VOLUME..............................................................................................................................5-31
5.5.18.2. MANUAL WEIGHT OR VOLUME..........................................................................................................................5-31
5.5.19. MAXIMUM TITRANT VOLUME.....................................................................................................................................5-31
5.5.20. POTENTIAL RANGE....................................................................................................................................................5-31
5.5.21. VOLUME/FLOW RATE................................................................................................................................................5-32
5.5.22. SIGNAL AVERAGING..................................................................................................................................................5-32
5.5.23. SIGNIFICANT FIGURES..............................................................................................................................................5-33
5.6. PRINTING...................................................................................................................................................................5-33
5.1. SELECTING METHODS
To select a method, press
from the main screen. A list of available methods will be displayed.
TITRATION METHODS
All of the 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
storage device.
In the Analysis 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.
5.2. 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.
5-3
TITRATION METHODS
5.2.1. 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 the 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).
5.2.2. 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 the Save to USB Storage Device 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
• Press
or
keys to remove unnecessary standard methods.
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).
5.2.3. RESTORE THE STANDARD METHODS TO THE MANUFACTURER SETTINGS
You can restore the standard methods to the default setting by highlighting a standard method and pressing
5-4
.
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.
5.3.1. CREATING USER METHODS
To create a new user method, start from a standard or user method and follow these steps:
• Press
• Using the
from the main screen.
and
keys, highlight an existing method from the method list.
• Press
. A new user method will be generated.
• Press
to activate the new user method.
TITRATION METHODS
5.3. USER METHODS
Note: Only a limited number of methods can be installed on the titrator. The titrator can hold 100 methods (standard and user).
When it is reached, a warning message will be displayed.
5.3.2. 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.
.
5-5
TITRATION METHODS
5.4. VIEW / MODIFY METHOD
To modify the method parameters, press
from the main screen. A list of all the parameters for the selected method will be
displayed. Using the
and
keys, highlight the option that you want to modify and choose
.
To exit the View / Modify Method screen, press
.
You can choose to save the modifications or to discard them.
5.5. METHOD OPTIONS
Note: Only certain method options can be changed for standard methods.
5.5.1. NAME
Option: Up to 24 characters
5-6
TITRATION METHODS
5.5.2. METHOD REVISION
Option: Up to 3 characters
5.5.3. STIRRER CONFIGURATION
Use the arrow keys to select the menu option.
5.5.3.1. STIRRER
Option: Stirrer 1 or Disabled 5-7
TITRATION METHODS
5.5.3.2. STIRRER SPEED
Option: 200 to 2500 RPM
5.5.4. PUMP CONFIGURATION
Option: Pump 1 or Pump 2 (if installed) 5-8
TITRATION METHODS
5.5.5. DOSING TYPE
Option: Linear or Dynamic
5.5.5.1. LINEAR DOSING
Linear dosing dispenses a pre-defined volume of titrant with every addition.
The Linear Dosing option is recommended for titrations with a slower reaction rate, difficult nonaqueous titrations, and specific
applications.
Note: For steep and normal titration curves, smaller volume increments are recommended, to obtain many points around the
equivalence point.
For flat titration curves, larger volume increments are recommended for equivalence point detection.
To set the dosing volume, select Linear Dosing and enter the optimum dose.
Dosing volume ranges are:
5 mL burette
0.001 to 4.750 mL
10 mL burette
0.001 to 9.500 mL
25 mL burette
0.005 to 23.750 mL
50 mL burette
0.005 to 47.500 mL
5-9
TITRATION METHODS
5.5.5.2. DYNAMIC DOSING
The titrator determines the titrant dose by trying to maintain a certain potential change (delta E) with each addition.
After a titrant dose, if the potential change is lower than the set delta E, the next dose will be progressively increased until max Vol is
attained. If the potential change is still lower than the set value, the titration will continue with max Vol doses.
After a titrant dose, if the potential change is higher than the set delta E, the next dose will be progressively decreased until min Vol
is attained. If the potential change is still higher than the set value, the titration will continue with min Vol doses.
The titrant is added in volumes that depend on the proximity of the end point as shown in the graph below.
Dynamic dosing allows for larger doses far from the end point, reducing the total titration time. Closer to the end point, smaller doses
are made, providing more data and improved accuracy.
The following parameters must be set:
min Vol: The smallest dose to be dispensed during a titration.
The min Vol must be greater than or equal to:
0.001 mL for a 5 mL burette
0.001 mL for a 10 mL burette
0.005 mL for a 25 mL burette
0.005 mL for a 50 mL burette
max Vol: The largest dose to be dispensed during a titration.
The max Vol must be less than or equal to 4.000 mL.
delta E: Sets the fixed potential jump that has to be achieved after each titrant dose.
The allowed range is between 0.1 and 99.999 mV.
Recommendations for dosing parameters:
For steep and normal titration curves the recommended settings are:
delta E
3.5
to 9 mV
min Vol
0.010
to 0.025 mL (for a 25 mL burette)
max Vol
0.075
to 0.250 mL (for a 25 mL burette)
For flat titration curves the recommended settings are:
delta E
10
to 15 mV
min Vol
0.050
to 0.150 mL (for a 25 mL burette)
max Vol
0.400
to 0.600 mL (for a 25 mL burette)
To achieve the highest levels of accuracy and reproducibility, it is recommended that 20-80% of the nominal burette volume used for
each titration is consumed. If lower volumes of titrant are required, a smaller burette can be used.
5-10
TITRATION METHODS
5.5.6. END POINT MODE
Option: Equivalence Point (pH or mV) or Fixed End Point (pH or mV)
5.5.6.1. FIXED END POINT (pH OR mV)
Fixed End Point (pH):
Option: -2.000 to 20.000 pH
The titration is terminated when the preset pH value has been exceeded. The end point volume is a calculated value based on the
dispensed volume when pH is under the preset value and the dispensed volume when pH exceeded the preset value.
5-11
TITRATION METHODS
Fixed End Point (mV):
Option: -2000.0 to 2000.0 mV
The end point detection algorithm is the same as for pH, but the threshold value is expressed in mV.
5.5.6.2. EQUIVALENCE END POINT (pH OR mV)
The titration is terminated when the equivalence point is detected (the point where the added quantity of titrant equals the quantity
of analyte present in the sample).
Number of Equivalence Points:
Option: 1 to 5
5-12
TITRATION METHODS
End Point Determination:
Option: 1st derivative or 2nd derivative
The equivalence point detection algorithm requires three additional titrant doses to be dispensed after the equivalence point is
reached.
The reported end point volume is a calculated value based on a number of points around the equivalence point.
The potentiometric titration curve is the response in mV potential or pH between the indication of the electrode versus the volume of
titrant added.
The inflection point of the titration curve is assumed to be the equivalence point of the chemical reaction.
For non-symmetric titration curves, the theoretical error can be reduced by using the dynamic dosing.
5-13
TITRATION METHODS
1st Derivative:
When first derivative is used to recognize the equivalence point, the titration curve inflection point (EQP) is the point where the first
derivative reaches its maximum value.
The detection algorithm looks for the maximum value of the first derivative. The first derivative must be greater than the threshold
value at the maximum point (see Recognition Options section).
2nd Derivative:
When second derivative is used to recognize the equivalence point, the titration curve inflection point (EQP) is the point where the
second derivative crosses zero.
The detection algorithm looks for the point where the second derivative changes sign.
The checked point, or first derivative, must be greater than the threshold value (see Recognition Options section).
5-14
The Recognition Options screen is a set of parameters used to avoid false detection of the equivalence point due to the chemical
system (titrant/sample species and concentrations) and/or electrode response.
TITRATION METHODS
5.5.7. RECOGNITION OPTIONS (EQUIVALENCE END POINT ONLY)
5.5.7.1. THRESHOLD
Option: 1 to 9999 mV/mL
This parameter must be set by the user according to the analysis.
The threshold represents the absolute value of the first derivative, expressed in mV/mL, below which the detection algorithm does not
search for the equivalence point.
The recommended value is 40% of the absolute value of the first derivative.
5-15
TITRATION METHODS
Depending on the titration curve profile, the following guide can be used:
TITRATION CURVE PROFILE
Flat
Normal
Steep
THRESHOLD (mV/mL)
1 to 450
50 to 1800
1800 to 9999
5.5.7.2. RANGE
Option: -2.000 to 20.000 pH or -2000.0 to 2000.0 mV
Range is an optional feature for equivalence point recognition. The titrator will only look for an equivalence point between the set
values.
The Range option can be enabled by selecting "Yes" in the Range Options screen.
5-16
TITRATION METHODS
The Limit 2 value must not be equal to the Limit 1 value.
5.5.7.3. FILTERED DERIVATIVES
Option: Yes or No
This option adds a filtering procedure in the 1st and 2nd derivative computation algorithm that reduces the influence of pH or mV
noise.
The Filtered Derivatives option can be enabled by selecting "Yes" in the Filtered Derivatives Option screen.
Noise can be due to:
•Chemical system properties (sample, titrant, solvent), such as slow chemical reactions or unbuffered samples such as
wastewater, tap water, wine
• Electrode response
• Incorrect method parameters settings such as Signal Stability, Stirring Speed, etc.
• Insufficient titrant additions
Note: A shift in the end point volume by 1 or 2 doses may be seen due to filtering.
5-17
TITRATION METHODS
5.5.8. PRE-TITRATION VOLUME
During a titration, the equivalence point is reached after many titrant doses. These doses take up extra time while having no
relevance for equivalence point detection.
Pre-titration volume adds a large initial dose to jump directly to the proximity of the equivalence point.
This first dose occurs after the pre-titration stir time is completed.
The ranges for pre-titration volumes are shown below:
0.001 to 4.750 mL for a 5 mL burette
0.001 to 9.500 mL for a 10 mL burette
0.005 to 23.750 mL for a 25 mL burette
0.005 to 47.500 mL for a 50 mL burette
To disable a pre-titration volume, enter 0.000 mL.
Note: A pre-titration volume is highly recommended whenever possible. Fewer doses will considerably shorten the overall titration
duration.
5.5.9. PRE-TITRATION STIR TIME
Option: 0 to 180 seconds
When enabled, the sample is mixed for a set period of time before any titrant is added. This allows the sample to become
homogeneous.
The Pre-Titration Stir Time option is disabled if 0 seconds is entered.
5-18
Option: Signal Stability or Timed Increment
During titration, the acquisition of the potential (mV) value of the solution can be done in two ways: Signal Stability or Timed
Increment option.
TITRATION METHODS
5.5.10. MEASUREMENT MODE
5.5.10.1. SIGNAL STABILITY
When signal stability is selected, the titrator acquires the potential (mV) only when stable conditions are reached.
The principles of signal stability are plotted below:
The signal stability window (condition) represents the time interval (∆t) during which the potential measured in solution (mV) is
confined inside the potential interval (∆E).
The new signal value is acquired if the stability condition is reached after the minimum (t min) wait time.
If the stability condition is not reached and the maximum (t max) wait time has elapsed, the potential is acquired.
5-19
TITRATION METHODS
delta E:
maximum change in potential during delta t
The range is from 0.1 to 99.9 mV.
delta t:
the time interval during which the potential is measured.
The range is from 1 to 10 seconds.
t min wait:
the minimum elapsed time before a stability check. This is also the minimum elapsed time between two doses.
The range is from 2 seconds to t max wait time.
t max wait:the maximum elapsed time between two successive doses. If the t max wait has elapsed, a new dose is added
even if the signal stability condition is not reached.
The range is from t min wait time to 180 seconds.
5.5.10.2. TIMED INCREMENT
Option: 2 to 180 seconds
When timed increment is selected, the titrator acquires the potential (mV) at a fixed time interval (no signal stability check).
The time period between two acquisitions must be set according to the reaction and the response time of the electrode.
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TITRATION METHODS
5.5.11. ELECTRODE TYPE
Option: Up to 20 characters
5.5.12. BLANK OPTION
Option: Disabled, V-Blank or Blank-V
This feature allows the user to select the procedure for the blank calculations (where V is the volume of titrant dispensed during the
titration and blank is the volume of titrant consumed by the blank sample).
5-21
TITRATION METHODS
If one of the options (V-Blank or Blank-V ) is selected in the View / Modify Method screen, the blank value will be active on the
View/Modify Method screen and the value of the blank can be set (in liters).
5.5.13. CALCULATIONS
The final result is calculated using the end point volume (titrant volume at the equivalence point or at the fixed end point), and a
formula selected by the user.
5.5.13.1. STANDARD TITRATION
5.5.13.1.1. EDIT VARIABLE VALUES
Edit the variables in a previously selected calculation.
For each formula, selected variables can be changed.
5.5.13.1.2. NO FORMULA (mL ONLY)
Only the volume of titrant (mL) required to reach the end point will be displayed.
5.5.13.1.3. NO FORMULA (L ONLY)
Only the volume of titrant (L) required to reach the end point is displayed.
5-22
This calculation is used when the concentration of an analyte is determined by the weight of the sample. The results are based on the
initial sample weight (in grams).
The titrator will calculate the results based on the selected units.
TITRATION METHODS
5.5.13.1.4. SAMPLE CALCULATIONS BY WEIGHT
The titrator will provide the results based on the titrant and sample units selected.
Titrant Units:
M (mol/L) moles/liter
N (eq/L) equivalents/liter
g/Lgrams/liter
mg/Lmilligrams/liter
Final Result Units:
ppt (g/kg) parts per thousand (grams/kilogram)
ppm (mg/kg) parts per million (milligrams/kilogram)
ppb (µg/kg) parts per billion (micrograms/kilogram)
% (g/100 g) percentage in weight (grams/100 grams)
mg/gmilligrams/gram
mg/kgmilligrams/kilogram
mol/kgmoles/kilogram
mmol/gmillimoles/gram
eq/kgequivalents/kilogram
meq/kgmilliequivalents/kilogram
5-23
TITRATION METHODS
A formula example is shown below using M (mol/L) as the titrant unit and ppt (g/kg) as the final result unit:
Variables can be set according to the amount of sample and titrant used.
5.5.13.1.5. SAMPLE CALCULATIONS BY VOLUME
This calculation is used when the concentration of an analyte is determined in terms of the volume of sample. The results are based
on the initial sample volume (in milliliters).
The titrator will calculate the results based on the selected units.
Titrant Units:
M (mol/L) moles/liter
N (eq/L) equivalents/liter
g/Lgrams/liter
mg/Lmilligrams/liter
5-24
TITRATION METHODS
Final Result Units:
ppt (g/L) parts per thousand (grams/liter)
ppm (mg/L) parts per million (milligrams/liter)
ppb (µg/L) parts per billion (micrograms/liter)
M (mol/L) Molarity (moles/liter)
N (eq/L) Normality (equivalents/liter)
mg/Lmilligrams/liter
µg/Lmicrograms/liter
mmol/Lmillimoles/liter
mg/mLmilligrams/milliliter
mg/100 mL milligrams/100 milliliters
g/100 mL grams/100 milliliters
eq/Lequivalents/liter
meq/Lmilliequivalents/liter
A formula example is shown below using N (eq/L) as the titrant units and g/L as the final result units:
Variables can be set according to the amount of sample and titrant used.
5.5.13.1.6. STANDARDIZE TITRANT BY WEIGHT
This calculation is used when the concentration of the titrant is determined using a solid standard. Determination of the titrant
concentration is based on the primary standard weight (in grams).
The calculation is based on the selected titrant unit. If the titrant unit is M (mol/L), the formula used to calculate the result is
displayed below:
5-25
TITRATION METHODS
5.5.13.1.7. STANDARDIZE TITRANT BY VOLUME
This calculation is used when the concentration of the titrant is determined using a primary standard solution. Determination of the
titrant concentration is based on the primary standard volume (in milliliters).
The calculation is based on the selected titrant unit. If the titrant unit is N (eq/L), the formula used to calculate the result is displayed
below:
5-26
The user can define their own calculation formula based on the final result units in a solid or liquid sample.
Final Result Units:
ppt (g/kg)
parts per thousand (grams/kilogram)
ppt (g/L)
parts per thousand (grams/liter)
ppm (mg/kg)
parts per million (milligrams/kilogram)
ppm (mg/L)
parts per million (milligrams/liter)
ppb (µg/kg) parts per billion (micrograms/kilogram)
ppb (µg/L)
parts per billion (micrograms/liter)
% (g/100 g)
percentage in weight (grams/100 grams)
M (mol/L)
Molarity (moles/liter)
mg/g milligrams/gram
N (eq/L)
Normality (equivalents/liter)
g/L gram/liter
mg/kg milligrams/kilogram
mg/L milligrams/liter
mol/kg moles/kilogram
µg/L micrograms/liter
mol/L moles/liter
mmol/g millimoles/gram
eq/kg equivalents/kilogram
mmol/L millimoles/liter
meq/kg milliequivalents/kilogram
mg/mL milligrams/milliliter
mg/100 mL
milligrams/100 milliliters
g/100 mL
grams/100 milliliters
eq/L equivalents/liter
meq/L milliequivalents/liter
No Unit
No result unit
The titrator will calculate the results based on the selected unit.
The formula can be either for titrant standardization or sample analysis.
TITRATION METHODS
5.5.13.1.8. GENERIC FORMULA
5-27
TITRATION METHODS
Where:
C= the concentration of the titrant
F1= general factor
F2= general factor
F3= general factor
S= sample size, in grams or milliliters
V= the volume delivered, in liters, to reach the preset or equivalence end point (determined by the titrator)
General factors:
Weight Conversion:
One of the general factors should be a weight conversion factor.
Examples of concentration units:
mol/L
eq/L
g/L
mg/L
moles/Liter
equivalents/Liter
grams/Liter
milligram/Liter
Reaction Ratio:
The reaction ratio is the ratio between the analyte and titrant or standard and titrant.
Examples of ratios:
mol/mol
moles of sample/moles of titrant
mol/eq
moles of sample/equivalents of titrant
eq/mol
equivalents of sample/moles of titrant
mol/mol
moles of titrant/moles of standard
eq/mol
equivalents of titrant/moles of standard
Example: 2 moles of NaOH react with 1 mole of H2SO4
Unit Conversion factor:
Used to convert between various measurement units.
Examples: L/1000 —> mL
g/1000 —> mg
Weight Conversion factor:
Used to convert between weight measurement bases (kg, g, mg, µg, mole or mmole).
Example: g —> mol
5-28
Final Dilution Volume:
Aliquot Volume:
Analyte size to be diluted:
TITRATION METHODS
5.5.14. DILUTION OPTION
Option: Enabled or Disabled
When the initial sample is diluted, a titration is made with an aliquot of the diluted sample, dilution calculations can be used.
The calculations are based on the original sample weight (volume) in order to express the results for the initial sample.
The volume of the sample after dilution
Volume of sample taken from the dilution for titration
The initial sample weight (volume)
5.5.15. TITRANT NAME
Option: Up to 15 characters
5-29
TITRATION METHODS
5.5.16. TITRANT CONCENTRATION
Enter the concentration of the titrant to be used. When determining the titrant concentration, only the concentration unit is displayed.
5.5.17. ANALYTE SIZE
Option: 0.001 to 250.0
Enter the size of the sample (for sample concentration determinations) or standard (for titrant concentration determination).
5.5.18. ANALYTE ENTRY
Option: Fixed or Manual
5-30
Each titration will use a set weight or volume in the calculations.
5.5.18.2. MANUAL WEIGHT OR VOLUME
Each titration, the exact weight or volume can be entered. The titrator will prompt for the analyte weight or volume at the beginning
of each titration.
5.5.19. MAXIMUM TITRANT VOLUME
TITRATION METHODS
5.5.18.1. FIXED WEIGHT OR VOLUME
Option: 0.100 to 100.000 mL
The maximum titrant volume used in the titration must be set according to the analysis.
If the titration end point (fixed or equivalence 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.
5.5.20. POTENTIAL RANGE
Option: -2000.0 to 2000.0 mV
The input potential range can be set by the user. The titration will be terminated and an error message will appear if the potential is
outside these limits.
These limits provide protection against a titration that does not generate an end point due to potential over-range.
5-31
TITRATION METHODS
5.5.21. VOLUME/FLOW RATE
The flow rate for the dosing system can be set by the user in an interval of 0.3 to two times the burette volume:
0.3 to 10 mL/min for a 5 mL burette
0.3 to 20 mL/min for a 10 mL burette
0.3 to 50 mL/min for a 25 mL burette
0.3 to 100 mL/min for a 50 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.
5.5.22. SIGNAL AVERAGING
Option: 1,2,3 or 4 readings
This option enables filtering on the mV/pH reading.
If 1 Reading is selected, the filtering is disabled. The titrator will take the last reading and place it into a “moving window” along with
the last 2, 3 or 4 readings (depending on the selected option). The average of those readings is displayed and used for calculations.
Averaging more readings is helpful when a noisy signal is received from the electrode.
5-32
Option: Two (XX), Three (XXX), Four (XXXX) or Five (XXXXX)
This option allows you to set the format for displaying the final titration result.
TITRATION METHODS
5.5.23. SIGNIFICANT FIGURES
5.6. 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 information about connecting a printer to the titrator).
5-33
5-34
6.1. RUNNING A TITRATION.............................................................................................................................................6-3
6.1.1. STARTING A TITRATION...............................................................................................................................................6-3
6.1.2. SUSPENDING A TITRATION..........................................................................................................................................6-3
6.1.3. VIEWING THE TITRATION CURVE..................................................................................................................................6-3
6.2. STOPPING A TITRATION............................................................................................................................................6-5
TITRATION MODE
CHAPTER 6. TITRATION MODE
6-1
6-2
Before beginning a titration, make sure that the following conditions are met:
• At least one pump is properly installed.
• A burette is inserted in the pump and filled with titrant.
•The aspiration tube is inserted in the titrant bottle and primed. The dispensing tube is over the titration beaker.
• The standard or sample has been carefully weighed/measured into the beaker.
• The electrode(s) and the temperature probe are submersed in the beaker.
• The desired method is selected and the parameters are set to the optimal values.
TITRATION MODE
6.1. RUNNING A TITRATION
6.1.1. STARTING A TITRATION
To start a new analysis, press
from the main screen.
When an analysis begins:
• The stirrer will turn on (if enabled).
•The pre-titration stir time starts, if enabled (see Titration Methods section).
•After the pre-titration stir time is complete the pre-titration volume will be displayed, if enabled. (see Titration Methods
section).
•The titrator will start the analysis and continue to deliver titrant until the end point is detected or the titration is terminated.
6.1.2. SUSPENDING A TITRATION
While a titration is in progress, you can temporarily stop it by pressing
To continue the titration press
.
. This will stop the dosing pump if it is running.
6.1.3. VIEWING THE TITRATION CURVE
During a titration, the potentiometric curve and the derivative curve (equivalence point only) can be displayed on the Titration
Graph screen by pressing
.
The potentiometric curve and the derivative curve are scaled to fit simultaneously inside the display.
When a titration end point is successfully detected, the volume is displayed on the graph and marked with an “x”.
6-3
TITRATION MODE
The contents of the graph as related to an end point type are as follows:
Equivalence End Point (pH): The pH readings and the selected derivative vs. volume of titrant are displayed (see Figure 1).
Equivalence End Point (mV): The mV readings and the selected derivative vs. volume of titrant are displayed (see Figure 2).
Fixed End Point (pH): The pH readings vs. volume of titrant are displayed (see Figure 3).
Fixed End Point (mV): The mV readings vs volume of titrant are displayed (see Figure 4).
Figure 1
Figure 2
Figure 3
Figure 4
- Changes the y-axis scale to either the mV (or pH) readings or the selected derivative values (of mV or pH). Available only
for titrations with equivalence end points.
- Allows you to save the graph as a bitmap file. Available only when the titration is finished.
6-4
The titration is terminated when one of the following conditions is met:
• Titration Completed: This is the only mode with valid final result values. The end point/stable reading was successfully
detected, the final results will be displayed.
•
Manually Terminated: The current titration terminated by the user before the end point was detected.
•
Limits Exceeded: The maximum titrant volume was delivered without reaching the end point. An error message is displayed on
the screen.
•
Critical Error: A critical error occurred and the titration was stopped. These errors are typically related to the dosing system. An
error message is displayed on the screen.
•
Potential Out of Range: The measured values from the electrode are outside the potential range. An error message is
displayed on the screen.
TITRATION MODE
6.2. STOPPING A TITRATION
6-5
6-6
7.1. DISPLAY.....................................................................................................................................................................7-3
7.2. pH SETUP...................................................................................................................................................................7-4
7.2.1. BUFFER ENTRY TYPE...................................................................................................................................................7-4
7.2.2. FIRST CALIBRATION POINT..........................................................................................................................................7-5
7.2.3. EDIT CUSTOM BUFFERS..............................................................................................................................................7-5
7.2.4. EDIT BUFFER GROUP..................................................................................................................................................7-6
7.2.5. CALIBRATION REMINDER.............................................................................................................................................7-7
7.2.6. SET REMINDER PERIOD...............................................................................................................................................7-7
7.2.7. CLEAR CALIBRATION...................................................................................................................................................7-8
7.2.8. pH GLP DATA..............................................................................................................................................................7-8
7.2.9. LOGGING INTERVAL.....................................................................................................................................................7-8
7.2.10. STABILITY CRITERIA..................................................................................................................................................7-9
7.2.11. pH RESOLUTION.......................................................................................................................................................7-9
7.2.12. STIRRER CONFIGURATION.........................................................................................................................................7-9
7.2.13. STIRRING SPEED......................................................................................................................................................7-10
7.3. pH CALIBRATION........................................................................................................................................................7-10
7.4. LOGGING....................................................................................................................................................................7-12
7.4.1. INTERVAL LOGGING.....................................................................................................................................................7-13
7.4.2. MANUAL LOGGING......................................................................................................................................................7-13
pH MODE
CHAPTER 7. pH MODE
7-1
7-2
pH MODE
By pressing
from the main screen, the titrator can be switched to Titrator, pH, mV or ISE modes.
One Analog Board
Switches to Titrator mode.
Switches to pH mode.
Switches to mV mode.
Switches to ISE mode.
7.1. DISPLAY
pH Mode Option keys:
T he General Options screen gives access to options that are not directly related to the measurement process (see
General Options section).
Stores the current pH reading (see Manual Logging section).
or
Starts the interval log (see Automatic Logging section).
Enter the pH calibration screen (see pH Calibration section).
Enter the pH setup screen, parameters are associated with pH measurements and calibration (see pH Setup section).
Allow the user to switch between the available measurement modes: Titrator, pH, mV or ISE mode.
7-3
pH MODE
7.2. pH SETUP
To access pH Setup, press
Use
Press
and
option key while in pH mode.
keys to highlight the desired option.
or
to access the selected option.
7.2.1. BUFFER ENTRY TYPE
Option: Automatic, Semiautomatic or Manual
Automatic: The instrument automatically selects the pH calibration point as the closest buffer from the predefined buffer group (see
Edit Buffer Group section).
Semiautomatic: The instrument automatically selects the closest buffer from the available buffers (standard and custom buffers).
Manual: The calibration buffer must be manually selected by the user during calibration from the available buffer list (standard and
custom buffers).
7-4
Option: Point or Offset
pH MODE
7.2.2. FIRST CALIBRATION POINT
If Point is selected, the slope values adjacent to the calibration points will be reevaluated (normal calibration).
If Offset is selected the existing slope values will not be changed.
7.2.3. EDIT CUSTOM BUFFERS
If you wish to use buffers other than the standard ones, use the Edit Custom Buffers option to set the desired pH value, up to five pH
custom buffers can be set.
Note: C ustom buffers are not temperature compensated, enter the value of the buffer at the calibration temperature.
• Use
and
keys to select the desired buffer.
• Press
to delete the selected buffer.
• Press
to edit the selected buffer.
7-5
pH MODE
• Use the numeric keypad to enter the pH buffer value.
• Press
• Press
to save the value.
to return to pH Setup menu.
7.2.4. EDIT BUFFER GROUP
Option: Up to five
Select up to five buffers from the available buffers (Hanna or Custom) to be used for automatic buffer recognition.
Within the buffer group, pH values must be at least 1.5 pH far apart.
If the buffer group already contains five pH buffers, at least one pH buffer has to be removed in order to add another buffer.
• Use the arrow keys to select the pH buffer to be included/removed in/from the buffer group.
• Press
or
to add/remove the selected pH buffer to/from buffer group.
• Press
7-6
to return to pH Setup menu.
pH MODE
7.2.5. CALIBRATION REMINDER
Option: Daily, Periodic or Disabled
Daily:
The calibration reminder will appear daily at a specified time.
Periodic: The calibration reminder will appear after the set time has elapsed since the last calibration.
Disabled: The calibration reminder will not appear.
7.2.6. SET REMINDER PERIOD
If Daily or Periodic option was selected for the calibration reminder, the reminder period must also be set.
For a daily reminder period, the time of day can be set.
For a periodic reminder period, the number of days, hours and minutes can be set.
• Press
to move the cursor to the next field.
• Press
to save the changes or
• Press
to disable the calibration reminder and return to pH setup.
to return to the previous screen.
7-7
pH MODE
7.2.7. CLEAR CALIBRATION
This option clears the existing pH calibration for the selected channel. If the calibration is cleared, the factory calibration will be used.
• Press
to clear the previous calibration or
to return to the previous screen without clearing the calibration.
7.2.8. pH GLP DATA
Displays the pH calibration data.
7.2.9. LOGGING INTERVAL
Option: 2 seconds to 8h 59 min 59 sec
Set the logging interval to be used for automatic logging.
7-8
Option: Fast, Medium, Accurate
pH MODE
7.2.10. STABILITY CRITERIA
Select the signal stability criteria:
Fast:
Quicker results with less accuracy
Medium: Medium speed results with medium accuracy
Accurate: Slower results with high accuracy
7.2.11. pH RESOLUTION
Option: One (X.X), Two (X.XX) or Three (X.XXX) decimal places
7.2.12. STIRRER CONFIGURATION
Option: Stirrer 1 or Disabled
7-9
pH MODE
7.2.13. STIRRING SPEED
Option: 200 to 2500 RPM
7.3. pH CALIBRATION
Calibrate the instrument often, especially if high accuracy is required.
The instrument should be recalibrated:
• Whenever the pH electrode is replaced.
• At least once a week.
• After testing aggressive chemicals.
• When “No pH Calibration” or “pH Calibration Expired” message appears on the display.
7-10
pH MODE
PREPARATION
Pour small quantities of the buffer solutions into clean beakers. If possible, use plastic beakers to minimize any EMC interferences.
For accurate calibration and to minimize cross-contamination, use two beakers for each buffer solution: one for rinsing the electrode
and one for calibration. If you are measuring in the acidic range, use pH 7.01 or 6.86 as the first buffer and pH 4.01/3.00 or 1.68
as the second buffer. If you are measuring in the alkaline range, use pH 7.01 or 6.86 as the first buffer and pH 10.01/9.18 or
12.45 as the second buffer.
For extended range measurements (acidic and alkaline), perform a five-point calibration by selecting five buffers across the entire pH
range.
CALIBRATION PROCEDURE
During calibration, the user has a choice of 8 standard buffers: (pH 1.68, 3.00, 4.01, 6.86, 7.01, 9.18, 10.01, 12.45) and up to 5
custom buffers.
For accurate measurements it is recommended to perform a five-point calibration. However, at least a two-point calibration is
suggested. For pH titrations, the selected buffers should bracket your end point (e.g.: if your end point value is at 8.5, use 7.01 or
6.86 and 9.18 or 10.01 for calibration).
To begin calibration:
• P ress
. If the instrument was calibrated before the old calibration can be cleared by pressing
.
Note: It is very important to clear calibration history when a new electrode is used.
• Immerse the pH electrode and the temperature probe approximately 4 cm (1.5”) into a buffer solution and stir gently.
• If necessary, select the pH calibration buffer value with
or
.
• O nce the reading has stabilized press
to update the calibration. The calibration buffer will be added to the Calibrated
Buffers section.
• R inse the pH electrode and the temperature probe, then immerse them into the next buffer solution and follow the above
procedure or press
to exit the calibration.
Notes:
• The new calibration points will replace old ones if the difference between them is ± 0.2 pH.
• Buffers used in older calibrations will not have a solid background.
• If calibrating with a standard buffer in MTC mode, the pH value and temperature can be modified by pressing
. The
values can be adjusted using the numeric keys. Press
to save the new values.
7-11
pH MODE
• In ATC mode, the pH value for custom buffers can be modified by pressing
.
• If the Automatic Buffer entry type was selected for the calibration procedure, the titrator will automatically select the closest
buffer to the measured pH value from the buffer group.
• If the Semiautomatic Buffer entry type was selected use the
or
to select the buffer. Only buffers in the
buffer group will be displayed.
CALIBRATION MESSAGES:
• W
rong Buffer. Please check the buffer: This message appears when the difference between the pH reading and the value of
the selected calibration buffer is significant. If the message is displayed, check if you have selected the appropriate calibration
buffer.
• Wrong buffer temperature: This message appears if the buffer temperature is out of the defined temperature range.
• Clean the electrode or check the buffer. Press
to update calibration: This message alerts the user that some dirt
or deposits could be on the electrode, or the buffer is contaminated.
• S lope too low. Please check the buffer: This message appears if the current slope is under 80% of the default slope.
Recalibrate the instrument using fresh buffers.
• S lope too high. Press
to clear the old calibration: This message appears as a result of an erroneous slope
condition.
7.4. LOGGING
Data logging is available in pH mode. It can be logging on demand (Manual Logging) or automatically (Interval Logging) at
predefined time intervals.
To customize the logging report:
• Press
to display the Data Parameters screen.
• Highlight the Setup pH/mV/ISE Report option and press
to display the Setup pH/mV/ISE Report screen.
• U se the
and
keys to highlight the data field that you want to show/hide in the pH/mV/ISE report and then press
to activate/deactivate it.
• E ach field marked by “*” is an active field selected for the report.
• P ress
to save the customized report.
7-12
The logging interval is set in the pH setup screen.
Press
to start the log.
The logging interval and name of logging file will be displayed on the pH measurement screen.
To stop the automatic logging, press
.
pH MODE
7.4.1. INTERVAL LOGGING
7.4.2. MANUAL LOGGING
To manually log pH readings, press
from the pH measurement screen.
A new record will be added to the report every time
is pressed.
7-13
7-14
8.1. DISPLAY.....................................................................................................................................................................8-3
8.2. mV SETUP...................................................................................................................................................................8-4
8.2.1. CLEAR RELATIVE mV OFFSET........................................................................................................................................8-4
8.2.2. LOGGING INTERVAL.....................................................................................................................................................8-4
8.2.3. STABILITY CRITERIA....................................................................................................................................................8-5
8.2.4. STIRRER CONFIGURATION...........................................................................................................................................8-5
8.2.5. STIRRING SPEED........................................................................................................................................................8-5
8.3. RELATIVE mV CALIBRATION.......................................................................................................................................8-6
8.4. LOGGING....................................................................................................................................................................8-6
8.4.1. INTERVAL LOGGING.....................................................................................................................................................8-7
8.4.2. MANUAL LOGGING......................................................................................................................................................8-7
mV MODE
CHAPTER 8. mV MODE
8-1
8-2
mV MODE
By pressing
from the main screen, the Titrator can be switched to Titrator, pH, mV or ISE modes.
One Analog Board
Switches to Titrator mode.
Switches to pH mode.
Switches to mV mode.
Switches to ISE mode.
8.1. DISPLAY
The mV screen is shown below.
mV Mode Option Keys:
T he General Options screen gives access to options that are not directly related to the measurement process (see
General Options section).
Stores the current mV reading (see Manual Logging section).
or
Starts the mV interval log (see Automatic Logging section).
Enter the mV calibration screen (see pH Calibration section).
Enter the mV setup screen, parameters are associated with pH measurements and calibration (see pH Setup section).
Allow the user to switch between the available measurement modes: Titrator, pH, mV or ISE mode.
8-3
mV MODE
8.2. mV SETUP
8.2.1. CLEAR RELATIVE mV OFFSET
Press
to clear the relative mV offset or
8.2.2. LOGGING INTERVAL
Option: 2 seconds to 8h 59min 59sec
8-4
to return to the previous screen.
Option: Fast, Medium or Accurate:
mV MODE
8.2.3. STABILITY CRITERIA
Fast:
Quicker results with less accuracy
Medium: Medium speed results with medium accuracy
Accurate: Slower results with high accuracy
8.2.4. STIRRER CONFIGURATION
Option: Stirrer 1 or Disabled
8.2.5. STIRRING SPEED
Option: 200 to 2500 RPM
8-5
mV MODE
8.3. RELATIVE mV CALIBRATION
• Press
to accept the value.
• Press
to cancel this operation and return to the previous screen.
• Press
to delete the last digit.
8.4. LOGGING
Data logging is available in mV mode. It can be logging on demand (Manual Logging) or automatically (Interval Logging) at
predefined time intervals.
To customize the logging report:
• Press
to display the Data Parameters screen.
• Highlight the Setup pH/mV/ISE Report option and press
•Use the
and
keys to highlight the data field that you want to show/hide in the pH/mV/ISE report and then press
to activate/deactivate it.
• Each field marked by “*” is an active field selected for the report.
• Press
8-6
to display the Setup pH/mV/ISE Report screen.
to save the customized report.
The logging interval is set in the mV Setup screen.
Press
to start the log.
The logging interval and name of logging file will be displayed on the measure screen.
To stop the automatic logging, press
again.
mV MODE
8.4.1. INTERVAL LOGGING
8.4.2. MANUAL LOGGING
To manually log mV readings, press
from the mV measurement screen.
A new record will be added to the report every time
is pressed.
8-7
8-8
9.1. DISPLAY.....................................................................................................................................................................9-3
9.2. ISE SETUP...................................................................................................................................................................9-4
9.2.1. CALIBRATION GROUP..................................................................................................................................................9-4
9.2.2. TEMPERATURE COMPENSATION...................................................................................................................................9-4
9.2.3. ISOPOTENTIAL POINT..................................................................................................................................................9-5
9.2.4. EDIT CUSTOM STANDARDS..........................................................................................................................................9-5
9.2.5. EDIT STANDARD GROUP..............................................................................................................................................9-6
9.2.6. CALIBRATION REMINDER.............................................................................................................................................9-6
9.2.7. SET REMINDER PERIOD...............................................................................................................................................9-7
9.2.8. CLEAR CALIBRATION...................................................................................................................................................9-7
9.2.9. ISE GLP DATA.............................................................................................................................................................9-8
9.2.10. ELECTRODE TYPE......................................................................................................................................................9-8
9.2.11. CONCENTRATION UNIT..............................................................................................................................................9-9
9.2.12. LOGGING INTERVAL...................................................................................................................................................9-10
9.2.13. STABILITY CRITERIA..................................................................................................................................................9-10
9.2.14. ISE SIGNIFICANT DIGITS............................................................................................................................................9-10
9.2.15. STIRRER CONFIGURATION.........................................................................................................................................9-11
9.2.16. STIRRING SPEED......................................................................................................................................................9-11
9.3. ISE CALIBRATION.......................................................................................................................................................9-11
9.4. LOGGING....................................................................................................................................................................9-12
9.4.1. INTERVAL LOGGING.....................................................................................................................................................9-13
9.4.2. MANUAL LOGGING......................................................................................................................................................9-13
ISE MODE
CHAPTER 9. ISE MODE
9-1
9-2
ISE MODE
By pressing
from the main screen, the Titrator can be switched to Titrator, pH, mV or ISE modes.
One Analog Board
Switches to Titrator mode.
Switches to pH mode.
Switches to mV mode.
Switches to ISE mode.
9.1. DISPLAY
The ISE screen is shown below.
ISE Mode option keys:
T he General Options screen gives access to options that are not directly related to the measurement process (see
General Options section).
Stores the current concentration reading (see Manual Logging section).
or
Starts the ISE interval log (see Interval Logging section).
Enter the ISE calibration screen (see ISE Calibration section).
Enter the ISE setup screen. Parameters are associated with ISE measurements and calibration.
Allows the user to switch between the available measurement modes: Titrator, pH, mV and ISE mode.
9-3
ISE MODE
9.2. ISE SETUP
To access the ISE Setup, press
option key in ISE mode.
9.2.1. CALIBRATION GROUP
Option: All Standards or Standards Group
All Standards:
The set of available standards includes the Standard solutions and Custom solutions.
Standards Group: The set of available standards includes only the standards selected by the user.
9.2.2. TEMPERATURE COMPENSATION
Option: Enabled or Disabled
Note: If you enabled Temperature Compensation, then the isopotential point must be set.
9-4
Option: 1.00 E-2 to 1.00 E+5 ppm
This option allows the user to set an isopotential point for the selected electrode when temperature compensation is enabled. The
isopotential point is edited in ppm units only. The isopotential point will vary for different electrodes, if measurements are going to be
made at several temperatures, the value should be entered if it is known.
ISE MODE
9.2.3. ISOPOTENTIAL POINT (TEMPERATURE COMPENSATION)
9.2.4. EDIT CUSTOM STANDARDS
Option: Up to five
• Use the
and
keys to select the standard.
• Press
to delete the standard.
• Press
to edit the selected custom standard; use the numeric keys to edit the standard.
9-5
ISE MODE
9.2.5. EDIT STANDARD GROUP
Option: Up to 5 standards
• Use the arrow keys to select the standard to be included/removed in/from the standard group.
• Press
or
to add/remove the selected standard to/from standard group.
• Press
to return to ISE Setup menu.
9.2.6. CALIBRATION REMINDER
Option: Daily, Periodic or Disabled
Daily:
Periodic:
Disable:
9-6
The calibration reminder will appear daily at specified time.
The calibration reminder will appear after the set time has elapsed since the last calibration.
The calibration reminder will not appear.
If Daily or Periodic option was selected for the calibration reminder, the reminder period must also be set.
For a daily reminder period the time of day can be set.
For a periodic reminder period the number of days, hours and minutes can be set.
•Press
to move the cursor to the next field.
•Press
to save the changes or
•Press
to disable the calibration reminder and return to ISE setup menu.
ISE MODE
9.2.7. SET REMINDER PERIOD
to return to the previous screen.
9.2.8. CLEAR CALIBRATION
This option clears the existing ISE calibration. If the calibration is cleared, a new calibration must be done in order to take
measurements.
•Press
to clear the previous calibration or
to return to the previous screen.
9-7
ISE MODE
9.2.9. ISE GLP DATA
Displays the ISE calibration data
9.2.10. ELECTRODE TYPE
Option: Ammonia, Bromide, Cadmium, Calcium, Carbon Dioxide, Chloride, Cupric, Cyanide, Fluoride, Iodide, Lead,
Nitrate, Potassium, Silver, Sodium, Sulfate, Sulfide or five custom electrodes
For Standard ISE:
•Press
screen.
9-8
to see the ion constants (name, molar weight, electric charge/slope), press
to return to the setup
•Press
•Use the
ISE MODE
For Custom ISE:
to edit the Ion constants for the selected custom ISE.
and
keys to highlight the desired ion constant and press
to edit the value.
•Set the Ion Name (up to 10 characters can be entered).
•Set the appropriate Molecular Weight (in g/mol) using the numeric keys. Press
return to the previous screen.
• S elect the appropriate Electric Charge/Slope. Use the
and
electric charge is none, manually set the slope by pressing
return to the previous screen.
to save the value or press
keys to select the value and then press
. Press
to save the value or press
to
. If the
to
9.2.11. CONCENTRATION UNIT
Options: ppt (g/L), ppm (mg/L), ppb (µg/L), mg/mL, M (mol/L), mmol/L, %w/v or user defined
9-9
ISE MODE
9.2.12. LOGGING INTERVAL
Option: 2 seconds to 8h 59 min 59 sec
9.2.13. STABILITY CRITERIA
Option: Fast, Medium, Accurate
Fast:
Quicker results with less accuracy
Medium: Medium speed results with medium accuracy
Accurate: Slower results with high accuracy
9.2.14. ISE SIGNIFICANT DIGITS
Option: One (X), Two (XX) or Three (XXX).
9-10
Option: Stirrer 1 or Disabled
ISE MODE
9.2.15. STIRRER CONFIGURATION
9.2.16. STIRRING SPEED
Option: 200 to 2500 RPM
9.3. ISE CALIBRATION
It is recommended to calibrate the instruments frequently if high accuracy is required. The instrument should also be recalibrated
whenever the “Calibrate Electrode” message appears on the LCD.
Due to electrode conditioning time, the electrode must be immersed for several seconds to stabilize. The user will be guided step by
step during calibration with easy-to-follow messages on the display. This will make the calibration a simple and error-free procedure.
PREPARATION:
Pour small quantities of the standard solution into clean beakers. If possible, use plastic beakers to minimize any EMC interferences.
For accurate calibration and to minimize cross-contamination, use two beakers for each standard solution: one for rinsing the
electrode and one for calibration.
Note: For accurate measurements, add the appropriate ISA (Ionic Strength Adjustment) to the calibration standards.
CALIBRATION PROCEDURE:
Before calibrating, make sure that the electrode type and concentration unit has been selected in ISE Setup.
Up to a five points calibration is possible using any combination of five standard solutions and five custom solutions.
The ISE calibration and measurement can be performed with or without temperature compensation. If the temperature compensation
option is enabled, the isopotential point of the electrode must be set in ISE Setup.
9-11
ISE MODE
•Press
from the main screen. If the instrument was calibrated before and the calibration was not cleared, the old
calibration can be cleared by pressing
.
•Immerse the ISE and the temperature probe approximately 2 cm into the standard with the lowest concentration.
• Select the standard concentration with
or
.
•When the reading has stabilized, press
Calibrated Standard list.
to update the calibration. The calibration point value will be added to the
• Select
and repeat the procedure with all of the available standards.
• Press
to exit the calibration.
9.4. LOGGING
Data logging is available in ISE mode. It can be logging on demand (Manual Logging) or automatically (Interval Logging) at
predefined time intervals.
To customize the logging report:
• Press
to display the Data Parameters screen.
• Highlight the Setup pH/mV/ISE Report option and press
•Use the
and
keys to highlight the data field that you want to show/hide in the pH/mV/ISE report and then press
to activate/deactivate it.
• Each field marked by “*” is an active field selected for the report.
9-12
• Press
to display the Setup pH/mV/ISE Report screen.
to save the customized report.
The logging interval is set in the ISE Setup screen.
Press
to start the log.
The logging interval and name of logging file will be displayed on the measure screen.
To stop the automatic logging, press
again.
ISE MODE
9.4.1. INTERVAL LOGGING
9.4.2. MANUAL LOGGING
To manually log ISE readings, press
from the ISE screen.
A new record will be added to the report every time
is pressed.
9-13
9-14
10.1. BURETTE...................................................................................................................................................................10-3
10.1.1. PRIME BURETTE.......................................................................................................................................................10-3
10.1.2. RINSE TIP................................................................................................................................................................10-4
10.1.3. MANUAL DISPENSE..................................................................................................................................................10-4
10.1.4. PURGE BURETTE.......................................................................................................................................................10-5
10.2. STIRRER....................................................................................................................................................................10-6
10.3. RESULTS...................................................................................................................................................................10-6
10.3.1. REVIEW LAST ANALYSIS REPORT................................................................................................................................10-6
10.3.1. REVIEW AVAILABLE REPORTS....................................................................................................................................10-7
10.3.1. GLP DATA.................................................................................................................................................................10-7
10.3.1. METER INFORMATION...............................................................................................................................................10-8
10.3.1. SETUP pH/mV/ISE REPORT.......................................................................................................................................10-9
10.3.1. SETUP TITRATION REPORT.........................................................................................................................................10-9
AUXILIARY FUNCTIONS
CHAPTER 10. AUXILIARY FUNCTIONS
10-1
10-2
To access the Burette screen, press
from the main titration screen.
Highlight the desired option and then press
.
AUXILIARY FUNCTIONS
10.1. BURETTE
allows you to select the desired pump for burette operations (it is only active if two pumps are connected).
10.1.1. PRIME BURETTE
Option: Up to 5
The Prime Burette option is used to fill the burette with titrant or reagent before starting a titration. The priming process consists of
several cycles of filling and emptying the burette with titrant.
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.
10-3
AUXILIARY FUNCTIONS
Note: Before starting this operation, the aspiration tube must be inserted in the titrant bottle. A waste container should be placed
under the dispensing tip to collect the waste solution.
To prime the burette, select Prime Burette, enter the number of rinses and press
.
We recommend at least three rinses to assure that the air bubbles are completely removed.
10.1.2. RINSE TIP
A 2 mL dose of titrant will be dispensed from the burette when this operation is selected, this will eliminate any air in the dispensing tip.
10.1.3. MANUAL DISPENSE
Manual Dispense option allows a defined titrant volume to be dosed. Select the Manual Dispense option and press
10-4
.
AUXILIARY FUNCTIONS
Use the numeric keypad to enter the volume to be dispensed.
The manual dispense volume must be between the limits shown below:
0.001 to 4.750 mL for a 5 mL burette
0.001 to 9.500 mL for a 10 mL burette
0.005 to 23.750 mL for a 25 mL burette
0.005 to 47.500 mL for a 50 mL burette
10.1.4. PURGE BURETTE
This option allows the burette to be emptied before cleaning and/or storing the burette. The burette is flushed twice.
Note: Before starting this operation, remove the aspiration tube from the titrant bottle.
The figures below show the steps in a purge burette operation.
10-5
AUXILIARY FUNCTIONS
10.2. STIRRER
The stirrer can be turned on and off by pressing
.
During the titration process, the stirring speed can be manually adjusted using the
and
keys.
10.3. RESULTS
From the Data Parameters screen, you can access the following options:
10.3.1. REVIEW LAST ANALYSIS REPORT
The information seen in the report is based on the selections made in the Setup Titration Report and Setup ISE/pH/mV Report
screen.
The following option keys are available:
Review the graph.
Print the titration report.
Return to the previous screen.
Keys can be used to scroll through the pages.
10-6
.
AUXILIARY FUNCTIONS
10.3.2. REVIEW 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 and Setup pH/mV/ISE Report screens during
report configuration.
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.
10.3.3. GLP DATA
Option: Up to 20 characters
10-7
AUXILIARY FUNCTIONS
Sample Name:Allows the sample name to be recorded in each report. The sample name will increase by one, with each new
titration or logging report, if the last character is a number.
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 Setup Titration Report screen (see Setup Titration Report section) in order to be displayed in the
titration report.
10.3.4. METER INFORMATION
Displays titrator configuration data.
Titrator Serial Number: The serial number of the titrator base board.
Analog Board 1 Serial Number: The serial number of the analog board.
Pump 1 (and/or 2) Serial Number: The serial number of the connected pump.
Titrator Software Version: The current software version installed on the titrator.
Base Board Software Version: The current software version present on the base board of the titrator.
Pump 1 (and/or 2) Software Version: The current software version for the pump.
Analog 1 Calibration Date: Manufacturer calibration date of the analog board.
Note: If more than 1 year elapsed from the calibration date of the analog board 1, the message Analog 1 Calibration Due
Calibration Due will appear on the main screen. The analog board needs to be recalibrated.
10-8
Customize a unique report to record the pH, mV, and ISE measurements. An asterisk means that it will be included in the report.
AUXILIARY FUNCTIONS
10.3.5. SETUP pH/mV/ISE REPORT
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.
10.3.6. SETUP TITRATION REPORT
Customize a unique report to record the titration results. An asterisk means that it will be included in the titration report.
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.
10-9
10-10
11.1. BURETTE MAINTENANCE..........................................................................................................................................11-3
11.1.1. BURETTE ASSEMBLY.................................................................................................................................................11-3
11.1.2. CHANGING THE BURETTE..........................................................................................................................................11-3
11.1.3. DISASSEMBLING THE BURETTE..................................................................................................................................11-3
11.1.4. ASSEMBLING THE BURETTE.......................................................................................................................................11-4
11.1.5. CLEANING THE BURETTE...........................................................................................................................................11-4
11.1.6. BURETTE PREPARATION (FILLING WITH TITRANT)........................................................................................................11-5
11.2. PERIPHERALS...........................................................................................................................................................11-6
11.2.1. CONNECTING TO A PRINTER.......................................................................................................................................11-6
11.2.2. CONNECTING AN EXTERNAL PC KEYBOARD..................................................................................................................11-6
11.2.3. CONNECTING TO A COMPUTER...................................................................................................................................11-8
MAINTENANCE PERIPHERALS
CHAPTER 11. MAINTENANCE, PERIPHERALS
11-1
11-2
11.1. BURETTE MAINTENANCE
11.1.1. BURETTE ASSEMBLY
The burette is delivered with a 25-mL syringe inside and with all of the accessories mounted (see Setup chapter). The burette
assembly consists of a rigid housing which holds the glass syringe, a 3-way valve and titrant tubing.
11.1.2. CHANGING THE BURETTE
Remove the burette from the pump assembly by sliding it forward and then slide the new burette into place.
MAINTENANCE PERIPHERALS
The 25-mL burette included with the titrator exceeds the ISO 8655 standard for accurate delivery of liquids by a motor-driven piston
burette.
11.1.3. DISASSEMBLING THE BURETTE
The aspiration and the dispensing tubes have fittings and tube protectors. The aspiration tube is mounted in the left side and the
dispensing tube is mounted in 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.
11-3
MAINTENANCE PERIPHERALS
11.1.4. ASSEMBLING THE BURETTE
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.
11.1.5. 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
chapter).
• Insert the aspiration tube into cleaning solution, deionized water or titrant solvent.
• Prime burette to fill the burette (use 2 rinses) (see Auxiliary Functions chapter).
•During second cycle remove the aspiration tube from the cleaning solution, deionized water or solvent and allow the air to
replace the liquid in the burette. This will clean the aspiration tube.
If this simple cleaning procedure is not adequate, continue with these steps:
• Remove the burette assembly from the pump.
• Remove the dispensing and aspiration tubes. Clean them separately or insert new ones.
• Remove the protective cap from the bottom of the burette assembly by using the burette removal tool.
• Remove the syringe from the burette assembly by unscrewing it with your fingers.
• Extract the piston from the syringe.
• Clean both the piston and the syringe with appropriate cleaning solution. Rinse with deionized water.
• Remove the excess liquid.
Warning: A void 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.
11-4
Reinsert the piston into the syringe.
Reinsert the syringe by screwing it in the valve with your fingers.
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. Notice the position of the piston shaft to the pump couple.
Priming the burette three times with new titrant is recommended.
MAINTENANCE PERIPHERALS
•
•
•
•
•
11.1.6. BURETTE PREPARATION (TITRANT FILLING)
Before starting a titration, the burette must be properly filled with titrant in order to obtain an accurate and repeatable result. 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 (minimum three rinses are recommend allowing air bubbles to be
evacuated).
• Press
.
To avoid the presence of the air bubbles inside the burette, make sure 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.
If air bubbles are still present:
• Remove the aspiration tube from the titrant bottle.
• Repeat burette preparation procedure.
• If this is not successful, clean the burette again.
11-5
MAINTENANCE PERIPHERALS
11.2. PERIPHERALS
Warning! C onnection/disconnection of POWER, PUMP ASSEMBLY, PRINTER, RS232 INTERFACE must only be done when
Titrator and external devices are turned off.
11.2.1. CONNECTING TO A PRINTER
A variety of parallel printers can be connected to the parallel port of the titrator using a DB25 cable.
Warning: T he titrator and the external printer must be both turned OFF before they are connected.
11.2.2. CONNECTING AN EXTERNAL PC KEYBOARD
This connection allows you to use an external PS/2 PC Keyboard in addition to the titrator’s keypad.
11-6
External PC Keyboard (United States 101)
Function Key F-1
Titrator Keypad
Function Key F-2
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
Function Key F-10
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)
MAINTENANCE PERIPHERALS
The correspondence between the titrator’s keypad and the United States 101-type external keyboard are:
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
Allow alphanumeric entries.
11-7
MAINTENANCE PERIPHERALS
11.2.3. 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.
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 Communication screen on the titrator (see General Options chapter)
Launch the HI900 PC application and then select the appropriate USB Port on the PC.
The HI900 PC application allows the transfer of methods and reports between the titrator and PC.
11-8
TECHNICAL SPECIFICATIONS
APPENDIX 1. TECHNICAL SPECIFICATIONS
A1 HI931 TECHNICAL SPECIFICATIONS............................................................................................................................A1-3
A1-1
A1-2
Analysis Type
End Point Mode
Burette
Stirrer
mV
pH
ISE
Temperature
Data Storage
Standard Titration (Standardization, Fixed pH/ mV, Equivalence Point pH/ mV)
Fixed mV
Fixed pH
mV Equivalence Point (1st or 2nd derivate)
pH Equivalence Point (1st or 2nd derivate)
Size
5 mL / 10 mL / 25 mL / 50 mL
Resolution
0.001 mL
Flow Rate
0.3 mL to 2 x Burette volume per minute
± 0.005 mL (5 mL Burette)
± 0.010 mL (10 mL Burette)
Accuracy
± 0.025 mL (25 mL Burette)
± 0.050 mL (50 mL Burette)
Range
200 to 2500 RPM
Resolution
100 RPM
Range
-2000.0 to 2000.0 mV
Resolution
0.1 mV
Accuracy
± 0.1 mV
Calibration
Single point offset
Range
-2.000 to 20.000 pH
Resolution
0.1 / 0.01 / 0.001 pH
Accuracy
± 0.001 pH
Calibration
Up to 5 points with standard or custom buffers
Range
1x10-6 to 9.999x1010
Resolution
1 / 0.1 / 0.01
Accuracy
± 0.001 pH
Calibration
Up to 5 points
-5.0 to 105 °C
Range
23.0 to 221.0 °F
268.2 to 378.2 K
Resolution
0.1 °C / 0.1 °F / 0.1 K
Accuracy
± 0.1 °C / ± 0.2 °F / ± 0.1 K
Methods
up to 100 titration methods (standard and user)
Reports
up to 100 titration and pH/mV/ISE reports
TECHNICAL SPECIFICATIONS
A1. HI931. TECHNICAL SPECIFICATIONS
A1-3
TECHNICAL SPECIFICATIONS
Connections
Additional
Specifications
A1-4
1 x BNC Socket (pH, ORP, ISE half-cell and ISE combination electrodes)
1 x 4 mm Banana Socket (reference electrode)
Measurement
1 x RCA Socket (temperature sensor)
1 x 6-pin Connector (stirrer)
1 x 6-pin Mini DIN (external PC keyboard)
1 x DB-25 Socket (printer)
Peripheral
1 x USB Standard B (PC connection)
1 x DB-9 Socket (analytical balance)
1 x USB Standard A (USB flash drive)
4 x multi-purpose slots (titrant/reagent tubes)
3 x 12-mm electrode slots
Electrode Holder
1 x temperature sensor slot
1 x overhead stirrer slot
Display
5.7" graphical color display with backlight
Languages
English, Portuguese, Spanish
Power Supply
100-240 Vac, 50/60 Hz
Power Draw
0.5 Amps
Enclosure Material ABS, PC and Stainless Steel
Keypad
Polyester
Dimensions
315 x 205 x 375 mm (12.4 x 8.1 x 14.8 ")
Weight
approx. 4.3 kg (9.5 lbs.) with 1 pump, stirrer and sensors
Operating
10 to 40 °C (50 to 104 °F); up to 95 % RH
Environment
Storage
-20 to 70 °C (-4 to 158 °F); up to 95 % RH
Environment
A2.1. SOLUTIONS..............................................................................................................................................................A2-3
A2.1.1. pH BUFFERS............................................................................................................................................................A2-3
A2.1.2. pH BUFFERS IN FDA APPROVED BOTTLE.....................................................................................................................A2-3
A2.1.3. pH TECHNICAL BUFFERS...........................................................................................................................................A2-3
A2.1.4. pH MILLESIMAL BUFFERS..........................................................................................................................................A2-3
A2.1.5. ELECTRODE CLEANING SOLUTIONS.............................................................................................................................A2-4
A2.1.6. ELECTRODE CLEANING SOLUTIONS IN FDA APPROVED BOTTLE......................................................................................A2-4
A2.1.7. ELECTRODE STORAGE SOLUTIONS..............................................................................................................................A2-4
A2.1.8. ELECTRODE STORAGE SOLUTIONS IN FDA APPROVED BOTTLE.......................................................................................A2-4
A2.1.9. ELECTRODE REFILL ELECTROLYTE SOLUTIONS..............................................................................................................A2-4
A2.1.10. ELECTRODE REFILL ELECTROLYTE SOLUTIONS IN FDA APPROVED BOTTLE.....................................................................A2-5
A2.1.11. ORP PRETREATMENT SOLUTIONS.............................................................................................................................A2-5
A2.1.12. TITRATION REAGENTS.............................................................................................................................................A2-5
A2.1.13. ION SELECTIVE ELECTRODE CALIBRATION STANDARDS...............................................................................................A2-5
A2.2 SENSORS...................................................................................................................................................................A2-6
A2.1.1. pH ELECTRODES.......................................................................................................................................................A2-6
A2.1.2. ORP ELECTRODES.....................................................................................................................................................A2-7
A2.1.3. HALF-CELL ELECTRODES............................................................................................................................................A2-7
A2.1.4. ION SELECTIVE ELECTRODES.....................................................................................................................................A2-8
A2.1.5. TEMPERATURE SENSOR............................................................................................................................................A2-8
A2.3. TITRATOR COMPONENTS.........................................................................................................................................A2-9
ACCESSORIES
APPENDIX 2. ACCESSORIES
A2-1
A2-2
A2.1.1. pH CALIBRATION BUFFERS
HI7001M
HI7001L
HI7004M
HI7004L
HI7006M
HI7006L
HI7007M
HI7007L
HI7009M
HI7009L
HI7010M
HI7010L
pH 1.68 Buffer Solution, 230 mL
pH 1.68 Buffer Solution, 500 mL
pH 4.01 Buffer Solution, 230 mL
pH 4.01 Buffer Solution, 500 mL
pH 6.86 Buffer Solution, 230 mL
pH 6.86 Buffer Solution, 500 mL
pH 7.01 Buffer Solution, 230 mL
pH 7.01 Buffer Solution, 500 mL
pH 9.18 Buffer Solution, 230 mL
pH 9.18 Buffer Solution, 500 mL
pH 10.01 Buffer Solution, 230 mL
pH 10.01 Buffer Solution, 500 mL
ACCESSORIES
A2.1. SOLUTIONS
A2.1.2. pH CALIBRATION BUFFERS IN FDA APPROVED BOTTLE
HI8004L
HI8006L
HI8007L
HI8009L
HI8010L
pH 4.01 Buffer Solution, 500 mL
pH 6.86 Buffer Solution, 500 mL
pH 7.01 Buffer Solution, 500 mL
pH 9.18 Buffer Solution, 500 mL
pH 10.01 Buffer Solution, 500 mL
A2.1.3. pH TECHNICAL CALIBRATION BUFFERS
HI5016
HI5003
HI5004
HI5068
HI5007
HI5091
HI5010
HI5124
pH 1.68 Buffer Solution, 500 mL
pH 3.00 Buffer Solution, 500 mL
pH 4.01 Buffer Solution, 500 mL
pH 6.86 Buffer Solution, 500 mL
pH 7.01 Buffer Solution, 500 mL
pH 9.18 Buffer Solution, 500 mL
pH 10.01 Buffer Solution, 500 mL
pH 12.45 Buffer Solution, 500 mL
A2.1.4. pH MILLESIMAL CALIBRATION BUFFERS
HI6016
HI6016-01
HI6003
HI6003-01
HI6004
HI6004-01
HI6068
HI6068-01
pH 1.679 Buffer Solution, 500 mL
pH 1.679 Buffer Solution, 1 L
pH 3.000 Buffer Solution, 500 mL
pH 3.000 Buffer Solution, 1 L
pH 4.010 Buffer Solution, 500 mL
pH 4.010 Buffer Solution, 1 L
pH 6.862 Buffer Solution, 500 mL
pH 6.862 Buffer Solution, 1 L
A2-3
ACCESSORIES
HI6007
HI6007-01
HI6091
HI6091-01
HI6010
HI6010-01
HI6124
HI6124-01
pH 7.010 Buffer Solution, 500 mL
pH 7.010 Buffer Solution, 1 L
pH 9.177 Buffer Solution, 500 mL
pH 9.177 Buffer Solution, 1 L
pH 10.010 Buffer Solution, 500 mL
pH 10.010 Buffer Solution, 1 L
pH 12.450 Buffer Solution, 500 mL
pH 12.450 Buffer Solution, 1 L
A2.1.5. ELECTRODE CLEANING SOLUTIONS
HI7061M
HI7061L
HI7073M
HI7073L
HI7074M
HI7074L
HI7077M
HI7077L
General Purpose Solution, 230 mL
General Purpose Solution, 500 mL
Protein Cleaning Solution, 230 mL
Protein Cleaning Solution, 500 mL
Inorganic Cleaning Solution, 230 mL
Inorganic Cleaning Solution, 500 mL
Oil & Fat Cleaning Solution, 230 mL
Oil & Fat Cleaning Solution, 500 mL
A2.1.6. ELECTRODE CLEANING SOLUTIONS IN FDA APPROVED BOTTLE
HI8061M
HI8061L
HI8073M
HI8073L
HI8077M
HI8077L
General Purpose Solution, 230 mL
General Purpose Solution, 500 mL
Protein Cleaning Solution, 230 mL
Protein Cleaning Solution, 500 mL
Oil & Fat Cleaning Solution, 230 mL
Oil & Fat Cleaning Solution, 500 mL
A2.1.7. ELECTRODE STORAGE SOLUTIONS
HI70300M
HI70300L
Storage Solution, 230 mL
Storage Solution, 500 mL
A2.1.8. ELECTRODE STORAGE SOLUTIONS IN FDA APPROVED BOTTLE
HI80300M
HI80300L
Storage Solution, 230 mL
Storage Solution, 500 mL
A2.1.9. ELECTRODE REFILL ELECTROLYTE SOLUTIONS
HI7071
3.5M KCl + AgCl Electrolyte, 30 mL, for single junction electrodes
HI7072
1M KNO3 Electrolyte, 30 mL
HI7075KNO3 and KCl Electrolyte, 30 mL
HI7076
1M NaCl Electrolyte, 30 mL
HI7078(NH4)2SO4 Electrolyte, 30 mL
HI7082
3.5M KCl Electrolyte, 30 mL, for double junction electrodes
A2-4
HI8071
HI8072
HI8082
3.5M KCl + AgCl Electrolyte, 30 mL, for single junction electrodes
1M KNO3 Electrolyte, 30 mL
3.5M KCl Electrolyte, 30 mL, for double junction electrodes
ACCESSORIES
A2.1.10. ELECTRODE REFILL ELECTROLYTE SOLUTIONS IN FDA APPROVED BOTTLE
A2.1.11. ORP PRETREATMENT SOLUTIONS
HI7091M
HI7091L
HI7092M
HI7092L
Reducing Pretreatment Solution, 230 mL
Reducing Pretreatment Solution, 500 mL
Oxidizing Pretreatment Solution, 230 mL
Oxidizing Pretreatment Solution, 500 mL
A2.1.12. TITRATION REAGENTS
HI70429
HI70433
HI70439
HI70440
HI70441
HI70448
HI70449
HI70455
HI70456
HI70457
HI70458
HI70459
HI70462
HI70463
HI70464
0.05 M AgNO3 Titration Reagent, 1 L
0.01 N Stabilized Iodine Titration Reagent, 1 L
0.1 M Na2S2O3 Titration Reagent, 1 L
0.02 N Stabilized Iodine Titration Reagent, 1 L
0.04 N Stabilized Iodine Titration Reagent, 1 L
0.02 M AgNO3 Titration Reagent, 1 L
0.02 M EDTA Titration Reagent, 1 L
0.01 N NaOH Titration Reagent, 1 L
0.1 N NaOH Titration Reagent, 1 L
1 N NaOH Titration Reagent, 1 L
0.01 M H2SO4 Titration Reagent, 1 L
0.05 M H2SO4 Titration Reagent, 1 L
0.01 N HCl Titration Reagent, 1 L
0.1 N HCl Titration Reagent, 1 L
1 N HCl Titration Reagent, 1 L
A2.1.13. ION SELECTIVE ELECTRODE CALIBRATION STANDARDS
HI4001-01
HI4001-02
HI4001-03
HI4002-01
HI4003-01
HI4004-01
HI4005-01
HI4005-03
HI4007-01
HI4007-02
HI4007-03
HI4008-01
0.1 M Ammonia Standard
100 ppm Ammonia Standard (as N)
1000 ppm Ammonia Standard (as N)
0.1 M Bromide Standard
0.1 M Cadmium Standard
0.1 M Calcium Standard
0.1 M Carbon Dioxide Standard
1000 ppm Carbon Dioxide Standard (as CaCO3)
0.1 M Chloride Standard
100 ppm Chloride Standard
1000 ppm Chloride Standard
0.1 M Cupric Standard
A2-5
ACCESSORIES
HI4010-01
HI4010-02
HI4010-03
HI4011-01
HI4012-01
HI4012-21
HI4013-01
HI4013-02
HI4013-03
HI4014-01
HI4015-01
0.1 M Fluoride Standard
100 ppm Fluoride Standard
1000 ppm Fluoride Standard
0.1 M Iodide Standard
0.1 M Lead Standard
0.1 M Sulfate Standard
0.1 M Nitrate Standard
100 ppm Nitrate Standard
1000 ppm Nitrate Standard
0.1 M Potassium Standard
0.1 M Silver Standard
A2.2. SENSORS
A2.2.1. pH ELECTRODES
HI1043B
Glass-body, double junction, refillable, combination pH electrode.
Use: strong acid and base, paint and solvents
HI1053B
Glass-body, triple ceramic, conic shape, refillable, combination pH electrode.
Use: emulsions, fats and creams, soil and semi-solids samples
HI1083B
Glass-body, micro, Viscolene, nonrefillable, combination pH electrode.
Use: biotechnology and micro titration
HI1131B
Glass-body, double junction, refillable, combination pH electrode.
Use: general purpose
HI1330B
Glass-body, semimicro, single junction, refillable, combination pH electrode.
Use: laboratory, vials, and test tubes
HI1331B
Glass-body, semimicro, single junction, refillable, combination pH electrode.
Use: flasks
HI1230B
Plastic-body (PEI), double junction, gel-filled, combination pH electrode.
Use: general purpose
HI2031B
Glass-body, conical tip, refillable, combination pH electrode.
Use: dairy and semi-solid products
HI1332B
Plastic-body (PEI), double junction, refillable, combination pH electrode.
A2-6
ACCESSORIES
Use: chemicals, field applications and quality control testing.
FC100B
Plastic-body (PVDF), double junction, refillable, combination pH electrode.
Use: cheese
FC200B
Plastic-body (PVDF), single junction, conical tip, non-refillable Viscolene electrolyte, combination pH electrode.
Use: milk, yogurt, dairy products, and semi-solid foods
FC210B
Glass-body, double junction, conical tip, non-refillable Viscolene electrolyte, combination pH electrode.
Use: milk, yogurt, and cream
FC220B
Glass-body, single junction, refillable, combination pH electrode.
Use: milk, yogurt, cream, sauce, and fruit juices
FC911B
Plastic-body (PVDF), double junction, refillable, combination pH electrode.
Use: sauce, juices, dairy products and other liquid or slurry forms of food
HI1413B
Glass-body, single junction, flat tip, non-refillable Viscolene electrolyte, combination pH electrode.
Use: surfaces, skin, leather, paper, and emulsions
A2.2.2. ORP ELECTRODES
HI3131B
Glass-body, refillable, combination platinum ORP electrode.
Use: laboratories and general purpose
HI3230B
Plastic-body (PEI), gel-filled, combination platinum ORP electrode.
Use: municipal water and quality control
HI4430B
Plastic-body (PEI), gel-filled, combination gold ORP electrode.
Use: oxidants and ozone
A2.2.3. HALF-CELL ELECTRODES
HI2110B
Glass-body, single half-cell pH electrode.
Use: general purpose
HI5311
Glass-body, Ag/AgCl reference half-cell electrode, double junction, refillable with 4mm banana plug with 1m (3.3’) cable.
Use: general purpose with wide temperature range
HI5315
Plastic-body (PEI), double junction, Ag/AgCl reference half-cell electrode, refillable with 4mm plug with 1 m (3.3’) cable.
Use: Ion Selective Electrodes
A2-7
ACCESSORIES
HI5412
Glass-body, single Calomel reference half-cell electrode, refillable with 4mm plug with 1m (3.3’) cable.
Use: general purpose with constant temperature range
A2.2.4. ION SELECTIVE ELECTRODES
HI4101 Ammonia ISE
HI4002 / HI4102 Bromide ISE
HI4003 / HI4103 Cadmium ISE
HI4004 / HI4104 Chloride ISE
HI4105 Carbon Dioxide ISE
HI4007 / HI4107 Chloride ISE
HI4008 / HI4108 Cupric ISE
HI4009 / HI4109 Cyanide ISE
HI4010 / HI4110 Fluoride ISE
HI4011 / HI4111 Iodide ISE
HI4012 / HI4112 Lead ISE
HI4013 / HI4113 Nitrate ISE
HI4014 / HI4114 Potassium ISE
HI4015 / HI4115 Silver / Sulfide ISE
FC300B Sodium
A2.2.5. TEMPERATURE SENSOR
HI7662-TW
Temperature probe with 1 m (3.3’) paneled cable.
A2-8
Pump Assembly
HI930100
Pump Assembly with Peristaltic Pump
HI930101
3 Way Valve
HI900260
Tool for burette cap removal
HI900942
Burette with:
5 mL syringe - HI930105
10 mL syringe - HI930110
25 mL syringe - HI930125
50 mL syringe - HI930150
5 mL Syringe
HI900205
10 mL Syringe
HI900210
25 mL Syringe
HI900225
50 mL Syringe
HI900250
ACCESSORIES
A2.3. TITRATOR COMPONENTS
Titrator Peristaltic Pump Complete
Tubing Set
HI930202
Aspiration Tube with fitting and
protection tube
HI900270
Dispensing Tube with normal dispensing
tip, fitting, protection tube and tube
guide
HI930280
Overhead Stirrer +
3 propellers
HI930301
Replacement Propellers
(3 pcs.)
HI930302
High Chemical Resistance Propellers
(3 pcs.)
HI930303
Stirrer Support
HI930320
A2-9
ACCESSORIES
Overhead Electrode Holder
HI930310
Temperature Probe
HI7662-TW
Power Adapter (USA Plug)
HI900946
Roller Tube for Titrator peristaltic pump
(3 pcs.)
HI930204
Power Adapter (European Plug)
HI900947
USB Cable
HI920013
USB Storage Device
HI930900U
Instruction Manual Binder
HI930800
Replacement Cap and Rotor
for Peristaltic Pump
HI930201
A2-10
Shorting Cap
HI900945
Blank Burette Support
HI930190
Blank Support
HI930191
Electrode adapter for
overhead stirrer holder
HI930311
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.
MAN931 10/18
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 HI931 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.
AUTOMATIC
POTENTIOMETRIC TITRATOR
GENERAL TITRATION APPLICATIONS BROCHURE
HI931
0.1N SODIUM HYDROXIDE TITRANT CONCENTRATION
DESCRIPTION
Method for the standardization (titer determination) of 0.1N Sodium
Hydroxide (NaOH) titrant solution against Potassium Hydrogen
Phthalate (KHP). The results are expressed in N (eq/L).
• R ecord the exact weight of the sample once the balance has
stabilized with an accuracy of 0.0001 grams.
• Remove the beaker from the balance and add deionized water
to the 50 mL mark on the beaker.
REFERENCE
AOAC Official Methods of Analysis, Official Method 936.16
ANALYSIS
• Place the beaker under the stirrer assembly and lower it to
immerse the pH electrode, temperature probe and stirrer. Ensure
that the reference junction of the pH electrode is 5 to 6 mm
below the surface. If necessary add extra deionized water.
Note: The dispensing tip should be slightly submerged in the
sample.
ELECTRODE
• H I1131B
• H I7662-T
Combination pH Electrode
Temperature Probe
REAGENTS
• H I70456
• H I70401
• H I70436
0.1N Sodium Hydroxide (1 L)
Potassium Hydrogen Phthalate (20 g)
Deionized Water (1 gal)
ACCESSORIES
• H I70300L Storage Solution (500 mL)
• H I7071
Electrode Fill Solution (30 mL x 4)
• H I7004L pH 4.01 Buffer Solution (500 mL)
• H I7007L pH 7.01 Buffer Solution (500 mL)
• H I7010L pH 10.01 Buffer Solution (500 mL)
• H I740036P 100 mL Plastic Beaker (10 pcs)
• A nalytical Balance with 0.0001 g resolution
DEVICE PREPARATION
• Connect the pH electrode and temperature probe to the titrator.
• Install a 25 mL burette filled with 0.1N sodium hydroxide
(HI70456) on pump one and verify that no air bubbles are present
in the burette or tubing. If necessary prime the burette until all the
air has been removed completely.
• P ress
from the main screen. Use the arrow keys
to highlight HI0001EN 0.1N Sodium Hydroxide and press
.
ELECTRODE PREPARATION
• Press
from the main screen, if necessary select the
analog board and press
.
• Calibrate the electrode using pH 4.01, 7.01 and 10.01 buffers.
Refer to the instruction manual for calibration procedure.
SAMPLE PREPARATION
• Crush approximately 3 grams of potassium hydrogen phthalate
(HI70401) and dry it for 2 hours at 120°C. Cool to room
temperature in a desiccator.
• P lace a clean 100 mL plastic beaker on the analytical balance.
• Z ero the balance.
• Carefully weigh approximately 0.20 grams of dried potassium
hydrogen phthalate into the beaker. Ensure that all of the
potassium hydrogen phthalate is on the bottom of the beaker.
• P ress
. You will be prompted to enter the weight of the
analyte (weight of potassium hydrogen phthalate). Use the
numeric keypad to enter the exact weight and press
to
start the analysis.
Note: Ensure that the potassium hydrogen phthalate dissolves
completely during the pre-titration stir time. Erroneous results
may occur if the sample does not dissolve completely prior to
titration. If necessary the pre-titration stir time can be increased.
• At the end of the titration, after detection of the equivalence
point, “Titration Completed” will appear with the result. The
result is expressed in N (eq/L) of sodium hydroxide.
• Remove the pH electrode, temperature probe and stirrer from the
sample and rinse them thoroughly with deionized water.
• R ecord the result.
Note: For improved accuracy, repeat this procedure a minimum
of three times and calculate the average value.
For methods utilizing 0.1N sodium hydroxide titrant solution,
follow the steps below to enter the titer/standardized value.
• S elect the method utilizing 0.1N sodium hydroxide.
• P ress
from the main screen.
• Using the arrow keys, highlight Titrant Conc. and press
.
• Use the numeric keypad to enter the standardized (titer) value
of the titrant then press
.
• P ress
to exit the View/Modify Method screen. Use
the arrow keys to highlight Save Method and press
.
0.1N SODIUM HYDROXIDE TITRANT CONCENTRATION
METHOD ID: HI0001EN
1
0.1N SODIUM HYDROXIDE TITRANT CONCENTRATION
2
METHOD ID: HI0001EN
0.1N SODIUM HYDROXIDE TITRANT CONCENTRATION
METHOD PARAMETERS
Name:
0.1N Sodium Hydroxide
Method Revision:
3.0
Analysis Type:
Standard Titration
Analog Board:
Analog 1
Stirrer Configuration:
Stirrer:
Stirrer 1
Stirring Speed:
1400 RPM
Pump Configuration:
Titrant Pump:
Pump 1
Reagent Addition 1:
Disabled
Reagent Addition 2:
Disabled
Dosing Type:
Dynamic
Min Vol:
0.030 mL
Max Vol:
0.500 mL
delta E:
4.500 mV
End Point Mode:
pH 1EQ point, 1st Der
Recognition Options:
Threshold:
500 mV/mL
Range:
NO
Filtered Derivatives:
NO
Pre-Titration Volume:
5.000 mL
Pre-Titration Stir Time:
60 sec
Measurement Mode:
Signal Stability
delta E:
0.3 mV
delta t:
2 sec
Min wait:
3 sec
Max wait:
30 sec
Electrode Type:
pH
Blank Option:
No Blank
Calculations:
Stdz. Titrant by Weight
Dilution Option:
Disabled
Titrant Name:
0.1N NaOH
Analyte Size:
0.20000 g
Analyte Entry:
Manual
Maximum Titrant Volume:
15.000 mL
Potential Range:
-2000.0 to 2000.0 mV
Volume/Flow Rate:
25 mL/50.0 mL/min
Signal Averaging:
1 Reading
Significant Figures:
XXXXX
CALCULATIONS
Calculations:
Stdz. Titrant by Weight
Titrant units:
N (eq/L)
Titrant volume dosed:
V (L)
Standard weight:
0.200 g
mw of standard:
204.23 g/mol
Titrant/Standard:
1.000 eq/mol
RESULTS
Titration Report
Method Name:
0.1N Sodium Hydroxide
Time & Date:
17:03 Jun 07, 2018
Report ID:
Ti_00053
Titration Results
Method Name:
0.1N Sodium Hydroxide
Time & Date:
17:03 Jun 07, 2018
Analyte Size:
0.20920 g
End Point Volume:
10.215 mL
pH Equivalence Point:
8.394
Result:
0.10027 N(eq/L)
Initial & Final pH:
4.173 to 9.570
Titration Duration:
6:25 [mm:ss]
Titration went to Completion
Analyst Signature:_____________________
0.1N HYDROCHLORIC ACID TITRANT CONCENTRATION
DESCRIPTION
Method for the standardization (titer determination) of 0.1N
Hydrochloric Acid (HCl) titrant solution against Sodium Hydroxide
(NaOH). The results are expressed in N (eq/L).
REFERENCE
AOAC Official Methods of Analysis, Official Method 936.15
ELECTRODE
• H I1131B
• H I7662-T
Combination pH Electrode
Temperature Probe
REAGENTS
• H I70463
• H I70456
• H I70436
0.1N Hydrochloric Acid (1 L)
0.1N Sodium Hydroxide (1 L)
Deionized Water (1 gal)
ACCESSORIES
• H I70300L Storage Solution (500 mL)
• H I7071
Electrode Fill Solution (30 mL x 4)
• H I7004L pH 4.01 Buffer Solution (500 mL)
• H I7007L pH 7.01 Buffer Solution (500 mL)
• H I7010L pH 10.01 Buffer Solution (500 mL)
• H I740036P 100 mL Plastic Beakers (10 pcs)
• 1 0 mL Class A Volumetric Pipette
• P ress
, the titrator start the analysis.
• At the end of the titration, after detection of the equivalence
point, “Titration Completed” will appear with the result. The
result is expressed in N (eq/L) of hydrochloric acid.
• Remove the pH electrode, temperature probe and stirrer from the
sample and rinse them thoroughly with deionized water.
• R ecord the result.
Note: For improved accuracy, repeat this procedure a minimum
of three times and calculate the average value.
For methods utilizing 0.1N hydrochloric acid titrant solution,
follow the steps below to enter the titer/standardized value.
• S elect the method utilizing 0.1N hydrochloric acid.
• P ress
from the main screen.
• Using the arrow keys, highlight Titrant Conc. and press
.
• Use the numeric keypad to enter the standardized (titer) value
of the titrant then press
.
• P ress
to exit the View/Modify Method screen. Use
the arrow keys to highlight Save Method and press
.
0.1N HYDROCHLORIC ACID TITRANT CONCENTRATION
METHOD ID: HI0002EN
DEVICE PREPARATION
• Connect the pH electrode and temperature probe to the titrator.
• Install a 25 mL burette filled with 0.1N hydrochloric acid (HI70463)
on pump one and verify that no air bubbles are present in the
burette or tubing. If necessary prime the burette until all the air has
been removed completely.
• P ress
from the main screen. Use the arrow keys
to highlight HI0002EN 0.1N Hydrochloric Acid and press
.
ELECTRODE PREPARATION
• Press
from the main screen and press
.
• Calibrate the electrode using pH 4.01, 7.01 and 10.01 buffers.
Refer to the instruction manual for calibration procedure.
SAMPLE PREPARATION
• Use a Class A volumetric pipette to transfer exactly 10.00 mL of
0.1N sodium hydroxide (HI70456) to a clean 100 mL beaker.
• A dd deionized water to the 50 mL mark on the beaker.
ANALYSIS
• Place the beaker under the stirrer assembly and lower it to
immerse the pH electrode, temperature probe and stirrer. Ensure
that the reference junction of the pH electrode is 5 to 6 mm
below the surface. If necessary add extra deionized water.
Note: The dispensing tip should be slightly submerged in the
sample.
3
0.1N HYDROCHLORIC ACID TITRANT CONCENTRATION
4
METHOD ID: HI0002EN
0.1N HYDROCHLORIC ACID TITRANT CONCENTRATION
METHOD PARAMETERS
Name:
0.1N Hydrochloric Acid
Method Revision:
3.0
Analysis Type:
Standard Titration
Analog Board:
Analog 1
Stirrer Configuration:
Stirrer:
Stirrer 1
Stirring Speed:
1400 RPM
Pump Configuration:
Titrant Pump:
Pump 1
Reagent Addition 1:
Disabled
Reagent Addition 2:
Disabled
Dosing Type:
Dynamic
Min Vol:
0.030 mL
Max Vol:
0.500 mL
delta E:
6.000 mV
End Point Mode:
pH 1EQ point, 1st Der
Recognition Options:
Threshold:
500 mV/mL
Range:
NO
Filtered Derivatives:
NO
Pre-Titration Volume:
5.000 mL
Pre-Titration Stir Time:
0 sec
Measurement Mode:
Signal Stability
delta E:
1.0 mV
delta t:
2 sec
Min wait:
3 sec
Max wait:
15 sec
Electrode Type:
pH
Blank Option:
No Blank
Calculations:
Stdz. Titrant by Volume
Dilution Option:
Disabled
Titrant Name:
0.1N HCl
Analyte Size:
10.0000 mL
Analyte Entry:
Fixed
Maximum Titrant Volume:
15.000 mL
Potential Range:
-2000.0 to 2000.0 mV
Volume/Flow Rate:
25 mL/50.0 mL/min
Signal Averaging:
1 Reading
Significant Figures:
XXXXX
CALCULATIONS
Calculations:
Stdz. Titrant by Volume
Titrant units:
N (eq/L)
Titrant volume dosed:
V (L)
Standard volume:
10.000 mL
Standard conc.:
0.100 eq/L
RESULTS
Titration Report
Method Name:
0.1N Hydrochloric Acid
Time & Date:
14:55 July 30, 2018
Report ID:
Ti_00002
Titration Results
Method Name:
0.1N Hydrochloric Acid
Time & Date:
14:55 July 30, 2018
Analyte Size:
10.000 mL
End Point Volume:
9.979 mL
pH Equivalence Point:
5.059
Result:
0.10020 N(eq/L)
Initial & Final pH:
12.135 to 4.989
Titration Duration:
2:45 [mm:ss]
Titration went to Completion
Analyst Signature:_____________________
0.1M SODIUM THIOSULFATE TITRANT CONCENTRATION
DESCRIPTION
Method for the standardization (titer determination) of 0.1M
Sodium Thiosulfate (Na2S2O3) titrant solution against Potassium
Iodate (KIO3). The results are expressed in M (mol/L).
REFERENCE
Standard Methods for the Examination of Water and Wastewater
19th Edition, Method 4500-Cl B
ELECTRODE
• HI3131B
Combination ORP Electrode
REAGENTS
• H I70439
• HI70407
• HI70425
• HI70468
• HI70436
0.1M Sodium Thiosulfate (1 L)
Potassium Iodate (20 g)
16% Sulfuric Acid (500 mL)
Potassium Iodide (35 g)
Deionized Water (1 gal)
ACCESSORIES
• H I70300L Storage Solution (500 mL)
• H I7071 Electrode Fill Solution (30 mL x 4)
• H I740036P 100 mL Plastic Beakers (10 pcs)
• A nalytical Balance 0.0001 g
• 1 00 mL Class A Volumetric Flask
• 1 0 mL Class A Volumetric Pipette
DEVICE PREPARATION
• Connect the ORP electrode to the titrator.
• Install a 25 mL burette filled with 0.1M sodium thiosulfate
(HI70439) on pump one and verify that no air bubbles are
present in the burette or tubing. If necessary prime the burette
until all the air has been removed completely.
• P ress
from the main screen. Use the arrow keys
to highlight HI0003EN 0.1M Sodium Thiosulfate and press
.
ELECTRODE PREPARATION
• Prepare the ORP electrode according to the procedure in the
manual.
SAMPLE PREPARATION
• Crush approximately 2 grams of potassium iodate (HI70407)
and dry it for 2 hours at 120°C. Cool to room temperature in a
desiccator.
• Carefully weigh approximately 0.35 grams of dried potassium
iodate.
• Record the exact weight of the sample once the balance has
stabilized with an accuracy of 0.0001 grams.
• Carefully transfer the salt to a 100 mL Class A volumetric flask.
Add approximately 80 mL of deionized water, and mix to
dissolve. Once the salt is completely dissolved bring the flask to
volume with deionized water, mix well.
• U se a Class A volumetric pipette to transfer exactly 10.00 mL of
the solution to a clean 100 mL plastic beaker.
• Add deionized water to the 50 mL mark on the beaker.
• Add 5.00 mL of 16% sulfuric acid (HI70425) and 1.5 grams of
potassium iodide (HI70468) to the beaker.
ANALYSIS
• Place the beaker under the stirrer assembly and lower it to
immerse the ORP electrode and stirrer. Ensure that the reference
junction of the ORP electrode is 5 to 6 mm below the surface. If
necessary add extra deionized water.
Note: The dispensing tip should be slightly submerged in the
sample.
• P ress
. You will be prompted to enter the weight of the
analyte (weight of potassium iodate). Use the numeric keypad
to enter the exact weight and press
to start the analysis.
• At the end of the titration, after detection of the equivalence
point, “Titration Completed” will appear with the result. The
result is expressed in M (mol/L) of sodium thiosulfate.
• Remove the ORP electrode and stirrer from the sample and rinse
them thoroughly with deionized water.
• R ecord the result.
Note: For improved accuracy, repeat this procedure a minimum
of three times and calculate the average value.
For methods utilizing 0.1M sodium thiosulfate titrant solution,
follow the steps below to enter the titer/standardized value.
• Select the method utilizing 0.1M sodium thiosulfate.
• P ress
from the main screen.
• Using the arrow keys, highlight Titrant Conc. and press
.
• Use the numeric keypad to enter the standardized (titer) value
of the titrant then press
.
• P ress
to exit the View/Modify Method screen. Use
the arrow keys to highlight Save Method and press
.
0.1M SODIUM THIOSULFATE TITRANT CONCENTRATION
METHOD ID: HI0003EN
5
0.1M SODIUM THIOSULFATE TITRANT CONCENTRATION
6
METHOD ID: HI0003EN
0.1M SODIUM THIOSULFATE TITRANT CONCENTRATION
METHOD PARAMETERS
Name:
0.1M Sodium Thiosulfate
Method Revision:
3.0
Analysis Type:
Standard Titration
Analog Board:
Analog 1
Stirrer Configuration:
Stirrer:
Stirrer 1
Stirring Speed:
1400 RPM
Pump Configuration:
Titrant Pump:
Pump 1
Reagent Addition 1:
Disabled
Reagent Addition 2:
Disabled
Dosing Type:
Dynamic
Min Vol:
0.030 mL
Max Vol:
0.600 mL
delta E:
6.500 mV
End Point Mode:
mV 1EQ point, 1st Der
Recognition Options:
Threshold:
50 mV/mL
Range:
NO
Filtered Derivatives:
NO
Pre-Titration Volume:
5.000 mL
Pre-Titration Stir Time:
0 sec
Measurement Mode:
Signal Stability
delta E:
0.3 mV
delta t:
2 sec
Min wait:
2 sec
Max wait:
20 sec
Electrode Type:
ORP
Blank Option:
No Blank
Calculations:
Stdz. Titrant by Weight
Dilution Option:
Enabled
Final Dilution Volume:
100.000 mL
Aliquot Volume:
10.000 mL
Titrant Name:
0.1M Na2S2O3
Analyte Size:
0.35000 g
Analyte Entry:
Manual
Maximum Titrant Volume:
15.000 mL
Potential Range:
-2000.0 to 2000.0 mV
Volume/Flow Rate:
25 mL/50.0 mL/min
Signal Averaging:
1 Reading
Significant Figures:
XXXXX
CALCULATIONS
Calculations:
Stdz. Titrant by Weight
Titrant units:
M (mol/L)
Titrant volume dosed:
V (L)
Standard weight:
0.350 g
Dilution Factor:
0.100
Final Dilution volume:
100.000 mL
Aliquot Volume:
10.000 mL
mw of standard:
214.00 g/mol
Titrant/Standard:
6.000 mol/mol
RESULTS
Titration Report
Method Name:
0.1M Sodium Thiosulfate
Time & Date:
17:10 Jun 22, 2018
Report ID:
Ti_00073
Titration Results
Method Name:
0.1M Sodium Thiosulfate
Time & Date:
17:10 Jun 22, 2018
Analyte Size:
0.35020 g
End Point Volume:
9.635 mL
mV Equivalence Point:
233.0
Result:
0.10191 M (mol/L)
Initial & Final mV:
361.8 to 173.4
Titration Duration:
2:51 [mm:ss]
Titration went to Completion
Analyst Signature:_____________________
0.1M FERROUS AMMONIUM SULFATE TITRANT CONCENTRATION
DESCRIPTION
Method for the standardization (titer determination) of 0.1M
Ferrous Ammonium Sulfate (FAS) titrant solution against Potassium
Dichromate (K2Cr2O7). The results are expressed in M (mol/L).
REFERENCE
Standard Methods for the Examination of Water and Wastewater
21st Edition, Method 5220B
ELECTRODE
• HI3131B
Combination ORP Electrode
REAGENTS
• H I70444 25% Sulfuric Acid
• H I70436 Deionized Water (1 gal)
• F errous Ammonium Sulfate (ACS Grade)
• P otassium Dichromate (ACS Grade)
ACCESSORIES
• H I70300L Storage Solution (500 mL)
• H I7071
Electrode Fill Solution (30 mL x 4)
• H I740036P 100 mL Plastic Beakers (10 pcs)
• A nalytical Balance with 0.0001 g resolution
• 1 00 mL Class A Volumetric Flask
• 5 00 mL Class A Volumetric Flask
• 1 0 mL Class A Volumetric Pipette
TITRANT PREPARATION
• Carefully weigh 19.607 grams of ferrous ammonium sulfate.
• Carefully transfer the salt to a 500 mL Class A volumetric flask. Add
approximately 300 mL of deionized water, and mix to dissolve.
• Add 40.00 mL of 25% sulfuric acid (HI70444) to the flask. Invert
the solution to mix.
• Allow the flask to return to room temperature.
• Bring the flask to volume with deionized water, mix well.
DEVICE PREPARATION
• Connect the ORP electrode to the titrator.
• Install a 25 mL burette filled with 0.1M ferrous ammonium
sulfate on pump one and verify that no air bubbles are present
in the burette or tubing. If necessary prime the burette until all
the air has been removed completely.
• P ress
from the main screen. Use the arrow keys to
highlight HI0010EN 0.1M FAS and press
.
ELECTRODE PREPARATION
• Prepare the ORP electrode according to the procedure in the
manual.
SAMPLE PREPARATION
• Crush approximately 2 grams of potassium dichromate and dry it
for 2 hours at 150°C. Cool to room temperature in a desiccator.
• C arefully weigh approximately 0.49 grams of dried potassium
dichromate.
• Record the exact weight of the sample once the balance has
stabilized with an accuracy of 0.0001 grams.
• Carefully transfer the salt to a 100 mL Class A volumetric flask.
Add approximately 80 mL of deionized water, and mix to
dissolve. Once the salt is completely dissolved bring the flask to
volume with deionized water, mix well.
• Use a Class A volumetric pipette to transfer exactly 10.00 mL of
the solution to a clean 100 mL plastic beaker.
• A dd 25.00 mL of 25% sulfuric acid (HI70444) to the beaker.
• A dd deionized water to the 50 mL mark on the beaker.
ANALYSIS
• Place the beaker under the stirrer assembly and lower it to
immerse the electrode and stirrer. Ensure that the reference
junction of the ORP electrode is 5 to 6 mm below the surface. If
necessary add extra deionized water.
Note: The dispensing tip should be slightly submerged in the
sample.
• P ress
. You will be prompted to enter the weight of the
analyte (weight of potassium dichromate). Use the numeric
keypad to enter the exact weight and press
to start the
analysis.
• At the end of the titration, after detection of the equivalence
point, “Titration Completed” will appear with the result. The
result is expressed in M (mol/L) of ferrous ammonium
sulfate.
• Remove the ORP electrode and stirrer from the sample and rinse
them thoroughly with deionized water.
• R ecord the result.
Note: For improved accuracy, repeat this procedure a minimum
of three times and calculate the average value.
For methods utilizing 0.1M ferrous ammonium sulfate titrant
solution, follow the steps below to enter the titer/standardized
value.
• Select the method utilizing 0.1M ferrous ammonium sulfate
• P ress
from the main screen.
• Using the arrow keys, highlight Titrant Conc. and press
.
• Use the numeric keypad to enter the standardized (titer) value
of the titrant then press
.
• P ress
to exit the View/Modify Method screen and
select Save Method and press
.
0.1M FERROUS AMMONIUM SULFATE TITRANT CONCENTRATION
METHOD ID: HI0010EN
7
0.1M FERROUS AMMONIUM SULFATE TITRANT CONCENTRATION
8
METHOD ID: HI0010EN
0.1M FERROUS AMMONIUM SULFATE TITRANT CONCENTRATION
METHOD PARAMETERS
Name:
0.1M FAS
Method Revision:
3.0
Analysis Type:
Standard Titration
Analog Board:
Analog 1
Stirrer Configuration:
Stirrer:
Stirrer 1
Stirring Speed:
1400 RPM
Pump Configuration:
Titrant Pump:
Pump 1
Reagent Addition 1:
Disabled
Reagent Addition 2:
Disabled
Dosing Type:
Dynamic
Min Vol:
0.030 mL
Max Vol:
0.500 mL
delta E:
4.500 mV
End Point Mode:
mV 1EQ point, 1st Der
Recognition Options:
Threshold:
35 mV/mL
Range:
NO
Filtered Derivatives:
NO
Pre-Titration Volume:
5.000 mL
Pre-Titration Stir Time:
0 sec
Measurement Mode:
Signal Stability
delta E:
0.5 mV
delta t:
3 sec
Min wait:
2 sec
Max wait:
20 sec
Electrode Type:
ORP
Blank Option:
No Blank
Calculations:
Stdz. Titrant by Weight
Dilution Option:
Enabled
Final Dilution Volume:
100.000 mL
Aliquot Volume:
10.000 mL
Titrant Name:
0.1M FAS
Analyte Size:
0.49000 g
Analyte Entry:
Manual
Maximum Titrant Volume:
15.000 mL
Potential Range:
-2000.0 to 2000.0 mV
Volume/Flow Rate:
25 mL/50.0 mL/min
Signal Averaging:
1 Reading
Significant Figures:
XXXXX
CALCULATIONS
Calculations:
Stdz. Titrant by Weight
Titrant units:
M (mol/L)
Titrant volume dosed:
V (L)
Standard weight:
0.490 g
Dilution Factor:
0.100
Final Dilution volume:
100.000 mL
Aliquot Volume:
10.000 mL
mw of standard:
294.18 g/mol
Titrant/Standard:
6.000 mol/mol
RESULTS
Titration Report
Method Name:
0.1M FAS
Time & Date:
15:59 August 1, 2018
Report ID:
Ti_00015
Titration Results
Method Name:
0.1M FAS
Time & Date:
15:59 August 1, 2018
Analyte Size:
0.491 g
End Point Volume:
9.879 mL
mV Equivalence Point:
667.4
Result:
0.10137 M (mol/L)
Initial & Final mV:
791.3 to 598.0
Titration Duration:
3:05 [mm:ss]
Titration went to Completion
Analyst Signature:_____________________
0.02M SILVER NITRATE TITRANT CONCENTRATION
DESCRIPTION
Method for the standardization (titer determination) of 0.02M Silver
Nitrate (AgNO3) titrant solution against Sodium Chloride (NaCl). The
results are expressed in M (mol/L).
REFERENCE
AOAC Official Methods of Analysis, Official Method 941.18
ELECTRODE
• HI4115
Silver/Sulfide Combination ISE
REAGENTS
• H I70448
• H I70406
• H I70427
• H I70436
0.02M Silver Nitrate (1 L)
Sodium Chloride (20 g)
1.5M Nitric Acid Solution (500 mL)
Deionized Water (1 gal)
ACCESSORIES
• H I7072
Electrode Fill Solution (4 x 30 mL)
• A nalytical Balance with 0.0001 g resolution
• 1 50 mL Glass Beaker
• 1 00 mL Class A Volumetric Flask
• 5 mL Class A Volumetric Pipette
DEVICE PREPARATION
• Connect the Silver/Sulfide electrode to the titrator.
• Install a 25 mL burette filled with 0.02M silver nitrate (HI70448)
on pump one and verify that no air bubbles are present in the
burette or tubing. If necessary prime the burette until all the air
has been removed completely.
• P ress
from the main screen. Use the arrow keys to
highlight HI0200EN 0.02M Silver Nitrate and press
.
ELECTRODE PREPARATION
• Prepare the Silver/Sulfide electrode according to the procedure in
the manual.
ANALYSIS
• Place the beaker under the stirrer assembly and lower it to
immerse the Silver/Sulfide electrode and stirrer. Ensure that
the reference junction of the electrode is 5 to 6 mm below the
surface. If necessary add extra deionized water.
Note: The dispensing tip should be slightly submerged in the
sample.
• P ress
. You will be prompted to enter the weight of the
analyte (weight of sodium chloride). Use the numeric keypad
to enter the exact weight and press
to start the analysis.
• At the end of the titration, after detection of the equivalence
point, “Titration Completed” will appear with the result. The
result is expressed in M (mol/L) of silver nitrate.
• Remove the electrode and stirrer from the sample and rinse them
thoroughly with deionized water.
• R ecord the result.
Note: For improved accuracy, repeat this procedure a minimum
of three times and calculate the average value.
For methods utilizing 0.02M silver nitrate titrant solution,
follow the steps below to enter the titer/standardized value.
• Select the method utilizing 0.02M silver nitrate.
• P ress
from the main screen.
• Using the arrow keys, highlight Titrant Conc. and press
.
• Use the numeric keypad to enter the standardized (titer) value
of the titrant then press
.
• P ress
to exit the View/Modify Method screen. Use
the arrow keys to highlight Save Method and press
.
0.02M SILVER NITRATE TITRANT CONCENTRATION
METHOD ID: HI0200EN
SAMPLE PREPARATION
• Crush approximately 2 grams of sodium chloride (HI70406)
and dry it for 2 hours at 140°C. Cool to room temperature in
a desiccator.
• Weigh 0.20 g of dried sodium chloride with an accuracy of
0.0001 g. Transfer the salt to a 100 mL volumetric flask.
Add approximately 80 mL of distilled water and mix. Dissolve
completely before bringing to volume.
• Use a Class A volumetric pipette to transfer exactly 5.00 mL of
prepared standard solution to a 150 mL glass beaker and add
distilled water to the 100 mL mark on the beaker.
• A dd 10.00 mL of 1.5M nitric acid (HI70427) to the beaker.
9
0.02M SILVER NITRATE TITRANT CONCENTRATION
10
METHOD ID: HI0200EN
0.02M SILVER NITRATE TITRANT CONCENTRATION
METHOD PARAMETERS
Name:
0.02M Silver Nitrate
Method Revision:
3.0
Analysis Type:
Standard Titration
Analog Board:
Analog 1
Stirrer Configuration:
Stirrer:
Stirrer 1
Stirring Speed:
1400 RPM
Pump Configuration:
Titrant Pump:
Pump 1
Reagent Addition 1:
Disabled
Reagent Addition 2:
Disabled
Dosing Type:
Dynamic
Min Vol:
0.030 mL
Max Vol:
0.500 mL
delta E:
8.000 mV
End Point Mode:
mV 1EQ point, 1st Der
Recognition Options:
Threshold:
100 mV/mL
Range:
NO
Filtered Derivatives:
YES
Pre-Titration Volume:
6.000 mL
Pre-Titration Stir Time:
0 sec
Measurement Mode:
Signal Stability
delta E:
1.0 mV
delta t:
2 sec
Min wait:
2 sec
Max wait:
20 sec
Electrode Type:
Silver/Sulfide
Blank Option:
No Blank
Calculations:
Stdz. Titrant by Weight
Dilution Option:
Enabled
Final Dilution Volume:
100.000 mL
Aliquot Volume:
5.000 mL
Titrant Name:
0.02M AgNO3
Analyte Size:
0.20000 g
Analyte Entry:
Manual
Maximum Titrant Volume:
15.000 mL
Potential Range:
-2000.0 to 2000.0 mV
Volume/Flow Rate:
25 mL/50.0 mL/min
Signal Averaging:
1 Reading
Significant Figures:
XXXXX
CALCULATIONS
Calculations:
Stdz. Titrant by Weight
Titrant units:
M (mol/L)
Titrant volume dosed:
V (L)
Standard weight:
0.200 g
Dilution Factor:
0.05
Final Dilution volume:
100.000 mL
Aliquot Volume:
5.000 mL
mw of standard:
58.440 g/mol
Titrant/Standard:
1.000 mol/mol
RESULTS
Titration Report
Method Name:
0.02M Silver Nitrate
Time & Date:
15:52 August 1, 2018
Report ID:
Ti_00037
Titration Results
Method Name:
0.02M Silver Nitrate
Time & Date:
15:52 August 1, 2018
Analyte Size:
0.1923 g
End Point Volume:
9.065 mL
mV Equivalence Point:
273.1
Result:
0.01815 M (mol/L)
Initial & Final mV:
146.9 to 291.0
Titration Duration:
2:21 [mm:ss]
Titration went to Completion
Analyst Signature:_____________________
ALKALINITY OF WATER
0 to 2500 mg/L CaCO3, pH 4.5 Endpoint
DESCRIPTION
Method for the determination of total (methyl red) alkalinity in
water by titration of a sample to pH 4.5. The results are expressed in
mg/L (ppm) as calcium carbonate.
For the determination of phenolphthalein alkalinity, set the endpoint
to pH 8.3.
REFERENCE
Standard Methods for the Examination of Water and Wastewater
21st edition, Method 2320B
ELECTRODE
• HI1131B
• HI7662-T
Combination pH Electrode
Temperature Probe
REAGENTS
• H I70463
• H I70436
0.1N Hydrochloric Acid (1 L)
Deionized Water (1 gal)
ANALYSIS
• Place the beaker under the stirrer assembly and lower it to
immerse the pH electrode, temperature sensor and stirrer.
Ensure that the reference junction of the pH electrode is 5 to 6
mm below the surface. If necessary add extra deionized water.
Note: The dispensing tip should be slightly submerged in the
sample.
ALKALINITY OF WATER
METHOD ID: HI1004EN
• P ress
, the titrator will start the analysis.
• At the end of the titration, when pH 4.50 is reached, “Titration
Completed” will appear with the result. The result is expressed
in mg/L as calcium carbonate.
• Remove the pH electrode, temperature probe and stirrer from the
sample and rinse them thoroughly with deionized water.
• R ecord the result.
ACCESSORIES
• H I70300L Storage Solution (500 mL)
• H I7082Electrode Fill Solution (4 x 30 mL)
• H I7004L pH 4.01 Buffer Solution (500 mL)
• H I7007L pH 7.01 Buffer Solution (500 mL)
• H I7010L pH 10.01 Buffer Solution (500 mL)
• H I740036P 100 mL Plastic Beaker (10 pcs)
• 5 0 mL Class A Volumetric Pipette
DEVICE PREPARATION
• Connect the pH electrode and temperature probe to the titrator.
• Install a 25 mL burette filled with 0.1N hydrochloric acid
(HI70463) on pump one and verify that no air bubbles are
present in the burette or tubing. If necessary prime the burette
until all the air has been removed completely.
• For the determination of the exact concentration of the 0.1N
hydrochloric acid, follow HI0002EN 0.1N Hydrochloric Acid
Titrant Concentration.
• P ress
from the main screen. Use the arrow keys to
highlight Alkalinity of Water and press
.
ELECTRODE PREPARATION
• Press
from the main screen, if necessary select the
analog board and press
.
• Calibrate the electrode using pH 4.01, 7.01 and 10.01 buffers.
Refer to the instruction manual for calibration procedure.
SAMPLE PREPARATION
• Use a Class A volumetric pipette to transfer exactly 50.00 mL of
sample to a clean 100 mL plastic beaker.
11
ALKALINITY OF WATER
12
METHOD ID: HI1004EN
ALKALINITY OF WATER
0 to 2500 mg/L CaCO3, pH 4.5 Endpoint
METHOD PARAMETERS
Name:
Alkalinity of Water
Method Revision:
3.0
Analysis Type:
Standard Titration
Analog Board:
Analog 1
Stirrer Configuration:
Stirrer:
Stirrer 1
Stirring Speed:
1400 RPM
Pump Configuration:
Titrant Pump:
Pump 1
Reagent Addition 1:
Disabled
Reagent Addition 2:
Disabled
Dosing Type:
Dynamic
Min Vol:
0.050 mL
Max Vol:
0.500 mL
delta E:
5.000 mV
End Point Mode:
Fixed 4.500 pH
Pre-Titration Volume:
0.000 mL
Pre-Titration Stir Time:
0 sec
Measurement Mode:
Signal Stability
delta E:
1.0 mV
delta t:
2 sec
Min wait:
2 sec
Max wait:
20 sec
Electrode Type:
pH
Blank Option:
No Blank
Calculations:
Sample Calc. by Volume
Dilution Option:
Disabled
Titrant Name:
0.1N HCl
Titrant Conc.:
0.1000 N(eq/L)
Analyte Size:
50.000 mL
Analyte Entry:
Fixed
Maximum Titrant Volume:
25.000 mL
Potential Range:
-2000.0 to 2000.0 mV
Volume/Flow Rate:
25 mL/50.0 mL/min
Signal Averaging:
1 Reading
Significant Figures:
XXXXX
CALCULATIONS
Calculations:
Sample Calc. by Volume
Titrant units:
N (eq/L)
Titrant volume dosed:
V (L)
Final result units:
mg/L
Titrant Conc.:
0.1000 N(eq/L)
Sample/Titrant:
0.500 mol/eq
mw of sample:
100.09 g/mol
Sample Volume:
50.000 mL
RESULTS
Titration Report
Method Name:
Alkalinity of Water
Time & Date:
14:36 August 1, 2018
Report ID:
Ti_00036
Titration Results
Method Name:
Alkalinity of Water
Time & Date:
14:36 August 1, 2018
Analyte Size:
50.000 mL
End Point Volume:
9.336 mL
pH Fixed End Point:
4.500
Result:
934.44 mg/L
Initial & Final pH:
10.232 to 4.419
Titration Duration:
3:23 [mm:ss]
Titration went to Completion
Analyst Signature:_____________________
ACIDITY OF WATER
0 to 2500 mg/L, pH 8.3 Endpoint
DESCRIPTION
Method for the determination of total (phenolphthalein) acidity in
water by titration of a sample to pH 8.3. The results are expressed in
mg/L (ppm) as calcium carbonate.
For the determination of methyl orange acidity, set the endpoint to
pH 3.7.
REFERENCE
Standard Methods for the Examination of Water and Wastewater
21st edition, Method 2310B
ELECTRODE
• HI1131B
• HI7662-T
Combination pH Electrode
Temperature Probe
REAGENTS
• H I70456
• H I70436
0.1N Sodium Hydroxide (1 L)
Deionized Water (1 gal)
ANALYSIS
• Place the beaker under the stirrer assembly and lower it to
immerse the pH electrode, temperature sensor and stirrer.
Ensure that the reference junction of the pH electrode is 5 to 6
mm below the surface. If necessary add extra deionized water.
Note: The dispensing tip should be slightly submerged in the
sample.
ACIDITY OF WATER
METHOD ID: HI1005EN
• P ress
, the titrator will start the analysis.
• At the end of the titration, when pH 8.30 is reached, “Titration
Completed” will appear with the result. The result is expressed
in mg/L as calcium carbonate.
• Remove the pH electrode, temperature probe and stirrer from the
sample and rinse them thoroughly with deionized water.
• R ecord the result.
ACCESSORIES
• H I70300L Storage Solution (500 mL)
• H I7082Electrode Fill Solution (4 x 30 mL)
• H I7004L pH 4.01 Buffer Solution (500 mL)
• H I7007L pH 7.01 Buffer Solution (500 mL)
• H I7010L pH 10.01 Buffer Solution (500 mL)
• H I740036P 100 mL Plastic Beaker (10 pcs)
• 5 0 mL Class A Volumetric Pipette
DEVICE PREPARATION
• Connect the pH electrode and temperature probe to the titrator.
• Install a 25 mL burette filled with 0.1N sodium hydroxide
(HI70456) on pump one and verify that no air bubbles are
present in the burette or tubing. If necessary prime the burette
until all the air has been removed completely.
• For the determination of the exact concentration of the 0.1N
sodium hydroxide, follow HI0001EN 0.1N Sodium Hydroxide
Titrant Concentration.
• P ress
from the main screen. Use the arrow keys to
highlight Acidity of Water and press
.
ELECTRODE PREPARATION
• Press
from the main screen, if necessary select the
analog board and press
.
• Calibrate the electrode using pH 4.01, 7.01 and 10.01 buffers.
Refer to the instruction manual for calibration procedure.
SAMPLE PREPARATION
• Use a Class A volumetric pipette to transfer exactly 50.00 mL of
sample to a clean 100 mL plastic beaker.
13
ACIDITY OF WATER
14
METHOD ID: HI1005EN
ACIDITY OF WATER
0 to 2500 mg/L, pH 8.3 Endpoint
METHOD PARAMETERS
Name:
Acidity of Water
Method Revision:
3.0
Analysis Type:
Standard Titration
Analog Board:
Analog 1
Stirrer Configuration:
Stirrer:
Stirrer 1
Stirring Speed:
1400 RPM
Pump Configuration:
Titrant Pump:
Pump 1
Reagent Addition 1:
Disabled
Reagent Addition 2:
Disabled
Dosing Type:
Dynamic
Min Vol:
0.050 mL
Max Vol:
0.500 mL
delta E:
5.000 mV
End Point Mode:
Fixed 8.300 pH
Pre-Titration Volume:
0.000 mL
Pre-Titration Stir Time:
0 sec
Measurement Mode:
Signal Stability
delta E:
1.0 mV
delta t:
2 sec
Min wait:
2 sec
Max wait:
20 sec
Electrode Type:
pH
Blank Option:
No Blank
Calculations:
Sample Calc. by Volume
Dilution Option:
Disabled
Titrant Name:
0.1N NaOH
Titrant Conc.:
0.1000 N(eq/L)
Analyte Size:
50.000 mL
Analyte Entry:
Fixed
Maximum Titrant Volume:
25.000 mL
Potential Range:
-2000.0 to 2000.0 mV
Volume/Flow Rate:
25 mL/50.0 mL/min
Signal Averaging:
1 Reading
Significant Figures:
XXXXX
CALCULATIONS
Calculations:
Sample Calc. by Volume
Titrant units:
N (eq/L)
Titrant volume dosed:
V (L)
Final result units:
(mg/L)
Titrant Conc.:
0.1000 N(eq/L)
Sample/Titrant:
0.500 mol/eq
mw of sample:
100.09 g/mol
Sample Volume:
50.000 mL
RESULTS
Titration Report
Method Name:
Acidity of Water
Time & Date:
14:54 August 1, 2018
Report ID:
Ti_00023
Titration Results
Method Name:
Acidity of Water
Time & Date:
14:54 August 1, 2018
Analyte Size:
50.000 mL
End Point Volume:
5.879 mL
pH Fixed End Point:
8.300
Result:
588.43 (mg/L)
Initial & Final pH:
2.465 to 8.398
Titration Duration:
3:42 [mm:ss]
Titration went to Completion
Analyst Signature:_____________________
CHLORIDE IN WATER
0 to 150 ppm (mg/L)
DESCRIPTION
Method for the determination of chloride in water. The results are
expressed as ppm (mg/L) as Chloride.
REFERENCE
Standard Methods for the Examination of Water and Wastewater
21st edition, Method 4500-Cl
ELECTRODE
• HI4115
Silver/Sulfide Combination ISE
REAGENTS
• HI70448
• HI70427
• HI70436
0.02M Silver Nitrate (1 L)
1.5M Nitric Acid Solution (500 mL)
Deionized Water (1 gal)
• P ress
, the titrator will start the analysis.
• At the end of the titration, after detection of the equivalence
point, “Titration Completed” will appear with the result. The
result is expressed in ppm (mg/L) of chloride.
• Remove the electrode and stirrer from the sample and rinse them
thoroughly with deionized water.
• R ecord the result.
CHLORIDE IN WATER
METHOD ID: HI1007EN
ACCESSORIES
• HI7072
Electrode Fill Solution (4 x 30 mL)
• 150 mL Glass Beaker
• 100 mL Class A Volumetric Pipette
• 10 mL Class A Volumetric Pipette
DEVICE PREPARATION
• Connect the Silver/Sulfide electrode to the titrator.
• Install a 25 mL burette filled with 0.02M silver nitrate (HI70448)
on pump one and verify that no air bubbles are present in the
burette or tubing. If necessary prime the burette until all the air
has been removed completely.
• For the determination of the exact concentration of the 0.02M
Silver Nitrate, follow HI0200EN 0.02M Silver Nitrate Titrant
Concentration
• P ress
from the main screen. Use the arrow keys to
highlight HI1007EN Chloride in Water and press
.
ELECTRODE PREPARATION
• Prepare the Silver/Sulfide electrode according to the procedure in
the manual.
SAMPLE PREPARATION
• Use a class A volumetric pipette to transfer exactly 100.00 mL of
sample to a clean 150 mL beaker.
• A dd 10.00 mL of 1.5M nitric acid (HI70427) to the beaker.
ANALYSIS
• Place the beaker under the stirrer assembly and lower it to
immerse the electrode and stirrer. Ensure that the reference
junction of the electrode is 5 to 6 mm below the surface. If
necessary add extra deionized water.
Note: The dispensing tip should be slightly submerged in the
sample.
15
CHLORIDE IN WATER
16
METHOD ID: HI1007EN
CHLORIDE IN WATER
0 to 150 ppm (mg/L)
METHOD PARAMETERS
Name:
Chloride in Water
Method Revision:
3.0
Analysis Type:
Standard Titration
Analog Board:
Analog 1
Stirrer Configuration:
Stirrer:
Stirrer 1
Stirring Speed:
1400 RPM
Pump Configuration:
Titrant Pump:
Pump 1
Reagent Addition 1:
Disabled
Reagent Addition 2:
Disabled
Dosing Type:
Dynamic
Min Vol:
0.030 mL
Max Vol:
0.500 mL
delta E:
5.000 mV
End Point Mode:
mv 1EQ point, 1st Der
Recognition Options:
Threshold:
100 mV/mL
Range:
NO
Filtered Derivatives:
NO
Pre-Titration Volume:
0.000 mL
Pre-Titration Stir Time:
0 sec
Measurement Mode:
Signal Stability
delta E:
1.0 mV
delta t:
2 sec
Min wait:
2 sec
Max wait:
20 sec
Electrode Type:
Silver/Sulfide
Blank Option:
No Blank
Calculations:
Sample Calc. by Volume
Dilution Option:
Disabled
Titrant Name:
0.02M AgNO3
Titrant Conc.:
2.0000E-2 M (mol/L)
Analyte Size:
100.0000 mL
Analyte Entry:
Manual
Maximum Titrant Volume:
25.000 mL
Potential Range:
-2000.0 to 2000.0 mV
Volume/Flow Rate:
25 mL/50.0 mL/min
Signal Averaging:
1 Reading
Significant Figures:
XXXXX
CALCULATIONS
Calculations:
Sample Calc. by Volume
Titrant units:
M (mol/L)
Titrant volume dosed:
V (L)
Titrant Conc.:
2.0000E-2 M (mol/L)
Sample/Titrant:
1.000 mol/mol
mw of sample:
35.453 g/mol
Sample Volume:
100.000 mL
RESULTS
Titration Report
Method Name:
Chloride in Water
Time & Date:
15:11 August 1, 2018
Report ID:
Ti_00052
Titration Results
Method Name:
Chloride in Water
Time & Date:
15:11 August 1, 2018
Analyte Size:
100.000 mL
End Point Volume:
4.781 mL
mV Equivalence Point:
280.3
Result:
33.897 ppm (mg/L)
Initial & Final mV:
194.8 to 298.5
Titration Duration:
1:24 [mm:ss]
Titration went to Completion
Analyst Signature:_____________________
NEUTRALIZATION WITH SULFURIC ACID
0 to 200 meq/L
DESCRIPTION
Method for the determination of strong or weak base concentration by
titration of a sample to the equivalence point with sulfuric acid. The
results are expressed as meq/L.
ELECTRODE
• HI1131B
• HI7662-T
REAGENTS
• HI70459
• HI70436
Combination pH Electrode
Temperature Probe
0.05M Sulfuric Acid (1 L)
Deionized Water (1 gal)
ACCESSORIES
• HI70300L Storage Solution (500 mL)
• HI7082Electrode Fill Solution (4 x 30 mL)
• HI7004L pH 4.01 Buffer Solution
• HI7007L pH 7.01 Buffer Solution
• HI7010L pH 10.01 Buffer Solution
• HI740036P 100 mL Plastic Beaker (10 pcs)
• 10 mL Class A Volumetric Pipette
ANALYSIS
• Place the beaker under the stirrer assembly and lower it to
immerse the pH electrode, temperature probe and stirrer. Ensure
that the reference junction of the pH electrode is 5 to 6 mm
below the surface.
Note: The dispensing tip should be slightly submerged in the
sample.
• P ress
, the titrator will start the analysis.
• At the end of the titration, after detection of the equivalence
point, “Titration Completed” will appear with the result. The
result is expressed in meq/L.
• Remove the pH electrode, temperature probe and stirrer from the
sample and rinse them thoroughly with deionized water.
• R ecord the result.
NEUTRALIZATION WITH SULFURIC ACID
METHOD ID: HI1008EN
DEVICE PREPARATION
• Connect the pH electrode and temperature probe to the titrator.
• Install a 25 mL burette filled with 0.05M sulfuric acid (HI70459)
on pump one and verify that no air bubbles are present in the
burette or tubing. If necessary prime the burette until all the air
has been removed completely.
• For the determination of the exact concentration of the 0.05M
sulfuric acid, follow HI0103EN 0.05M Sulfuric Acid Titrant
Concentration.
• P ress
from the main screen. Use the arrow keys
to highlight HI1008EN Neutralization w/H2SO4 and press
.
ELECTRODE PREPARATION
• Press
from the main screen, if necessary select the
analog board and press
.
• Calibrate the electrode using pH 4.01, 7.01 and 10.01 buffers.
Refer to the instruction manual for calibration procedure.
SAMPLE PREPARATION
• Use a class A volumetric pipette to transfer exactly 10.00 mL of
sample to a clean 100 mL plastic beaker.
• A dd deionized water to the 50 mL mark on the beaker.
17
NEUTRALIZATION WITH SULFURIC ACID
18
METHOD ID: HI1008EN
NEUTRALIZATION WITH SULFURIC ACID
0 to 200 meq/L
METHOD PARAMETERS
Name:
Neutralization w/ H2S04
Method Revision:
3.0
Analysis Type:
Standard Titration
Analog Board:
Analog 1
Stirrer Configuration:
Stirrer:
Stirrer 1
Stirring Speed:
1400 RPM
Pump Configuration:
Titrant Pump:
Pump 1
Reagent Addition 1:
Disabled
Reagent Addition 2:
Disabled
Dosing Type:
Dynamic
Min Vol:
0.050 mL
Max Vol:
0.500 mL
delta E:
20.000 mV
End Point Mode:
pH 1EQ point, 1st Der
Recognition Options:
Threshold:
50 mV/mL
Range:
NO
Filtered Derivatives:
NO
Pre-Titration Volume:
0.000 mL
Pre-Titration Stir Time:
0 sec
Measurement Mode:
Signal Stability
delta E:
1.0 mV
delta t:
2 sec
Min wait:
2 sec
Max wait:
15 sec
Electrode Type:
pH
Blank Option:
No Blank
Calculations:
Sample Calc. by Volume
Dilution Option:
Disabled
Titrant Name:
0.05M H2S04
Titrant Conc.:
5.0000E-2 M (mol/L)
Analyte Size:
10.000 mL
Analyte Entry:
Fixed
Maximum Titrant Volume:
20.000 mL
Potential Range:
-2000.0 to 2000.0 mV
Volume/Flow Rate:
25 mL/50.0 mL/min
Signal Averaging:
1 Reading
Significant Figures:
XXXXX
CALCULATIONS
Calculations:
Sample Calc. by Volume
Titrant units:
M (mol/L)
Titrant volume dosed:
V (L)
Final result units:
meq/L
Titrant Conc.:
5.0000E-2 M (mol/L)
Sample/Titrant:
2.000 eq/mol
Sample Volume:
10.000 mL
RESULTS
Titration Report
Method Name:
Neutralization w/ H2SO4
Time & Date:
09:46 August 1, 2018
Report ID:
Ti_00027
Titration Results
Method Name:
Neutralization w/ H2SO4
Time & Date:
09:46 August 1, 2018
Analyte Size:
10.000 mL
End Point Volume:
9.562 mL
pH Equivalence Point:
7.966
Result:
95.620 meq/L
Initial & Final pH:
11.655 to 6.248
Titration Duration:
3:26 [mm:ss]
Titration went to Completion
Analyst Signature:_____________________
NEUTRALIZATION WITH SODIUM HYDROXIDE
0 to 200 meq/L
DESCRIPTION
Method for the determination of strong or weak acid concentration by
titration of a sample to the equivalence point with sodium hydroxide.
The results are expressed as meq/L.
ELECTRODE
• HI1131B
• HI7662-T
REAGENTS
• HI70456
• HI70436
Combination pH Electrode
Temperature Probe
0.1N Sodium Hydroxide (1 L)
Deionized Water (1 gal)
ACCESSORIES
• HI70300L Storage Solution (500 mL)
• HI7082Electrode Fill Solution (4 x 30 mL)
• HI7004L pH 4.01 Buffer Solution
• HI7007L pH 7.01 Buffer Solution
• HI7010L pH 10.01 Buffer Solution
• HI740036P 100 mL Plastic Beakers (10 pcs)
• 10 mL Class A Volumetric Pipette
ANALYSIS
• Place the beaker under the stirrer assembly and lower it to
immerse the pH electrode, temperature probe and stirrer. Ensure
that the reference junction of the pH electrode is 5 to 6 mm
below the surface.
Note: The dispensing tip should be slightly submerged in the
sample.
• P ress
, the titrator will start the analysis.
• At the end of the titration, after detection of the equivalence
point, “Titration Completed” will appear with the result. The
result is expressed in meq/L.
• Remove the pH electrode, temperature sensor and stirrer from
the sample and rinse them thoroughly with deionized water.
• R ecord the result.
NEUTRALIZATION WITH SODIUM HYDROXIDE
METHOD ID: HI1009EN
DEVICE PREPARATION
• Connect the pH electrode and temperature probe to the titrator.
• Install a 25 mL burette filled with 0.1N sodium hydroxide
(HI70456) on pump one and verify that no air bubbles are
present in the burette or tubing. If necessary prime the burette
until all the air has been removed completely.
• For the determination of the exact concentration of the 0.1N
sodium hydroxide, follow HI0001EN 0.1N Sodium Hydroxide
Titrant Concentration.
• P ress
from the main screen. Use the arrow keys
to highlight HI1009EN Neutralization w/NaOH and press
.
ELECTRODE PREPARATION
• Press
from the main screen, if necessary select the
analog board and press
.
• Calibrate the electrode using pH 4.01, 7.01 and 10.01 buffers.
Refer to the instruction manual for calibration procedure.
SAMPLE PREPARATION
• Use a class A volumetric pipette to transfer exactly 10.00 mL of
sample to a clean 100 mL plastic beaker.
• A dd deionized water to the 50 mL mark on the beaker.
19
NEUTRALIZATION WITH SODIUM HYDROXIDE
20
METHOD ID: HI1009EN
NEUTRALIZATION WITH SODIUM HYDROXIDE
0 to 200 meq/L
METHOD PARAMETERS
Name:
Neutralization w/ NaOH
Method Revision:
3.0
Analysis Type:
Standard Titration
Analog Board:
Analog 1
Stirrer Configuration:
Stirrer:
Stirrer 1
Stirring Speed:
1400 RPM
Pump Configuration:
Titrant Pump:
Pump 1
Reagent Addition 1:
Disabled
Reagent Addition 2:
Disabled
Dosing Type:
Dynamic
Min Vol:
0.050 mL
Max Vol:
0.500 mL
delta E:
20.000 mV
End Point Mode:
pH 1EQ point, 1st Der
Recognition Options:
Threshold:
50 mV/mL
Range:
NO
Filtered Derivatives:
NO
Pre-Titration Volume:
0.000 mL
Pre-Titration Stir Time:
0 sec
Measurement Mode:
Signal Stability
delta E:
1.0 mV
delta t:
2 sec
Min wait:
2 sec
Max wait:
15 sec
Electrode Type:
pH
Blank Option:
No Blank
Calculations:
Sample Calc. by Volume
Dilution Option:
Disabled
Titrant Name:
0.1N NaOH
Titrant Conc.:
0.1000 N(eq/L)
Analyte Size:
10.000 mL
Analyte Entry:
Fixed
Maximum Titrant Volume:
20.000 mL
Potential Range:
-2000.0 to 2000.0 mV
Volume/Flow Rate:
25 mL/50.0 mL/min
Signal Averaging:
1 Reading
Significant Figures:
XXXXX
CALCULATIONS
Calculations:
Sample Calc. by Volume
Titrant units:
N (eq/L)
Titrant volume dosed:
V (L)
Final result units:
meq/L
Titrant Conc.:
0.1000 N(eq/L)
Sample Volume:
10.000 mL
RESULTS
Titration Report
Method Name:
Neutralization w/ NaOH
Time & Date:
10:29 August 2, 2018
Report ID:
Ti_00017
Titration Results
Method Name:
Neutralization w/ NaOH
Time & Date:
10:29 August 2, 2018
Analyte Size:
10.000 mL
End Point Volume:
15.970 mL
pH Equivalence Point:
8.431
Result:
159.70 meq/L
Initial & Final pH:
2.675 to 10.316
Titration Duration:
3:20 [mm:ss]
Titration went to Completion
Analyst Signature:_____________________
TROUBLESHOOTING 1
DESCRIPTION
Method for verifying the dosing and potentiometric signal accuracy
of the titrator. This method should be used to troubleshoot a titrator
equipped with a 25 mL burette. The titrator dispenses a 20.00 mL
pre-titration volume, waits 20 seconds and dispenses an additional
20.00 mL dose, bringing the total volume to 40.00 mL. This
procedure can also be used to check the stability of the mV and
temperature channels.
The specifications of the dosing accuracy are ± 0.1% of the full
burette volume (± 0.025 mL for a 25 mL burette). For the accuracy
of other burette volumes, see the instruction manual.
If the results are not correct, check all fittings for leakage, and burette
and tubing for air bubbles. Repeat the measurement.
• T he following information is needed to verify the accuracy of the
dosing system:
• T he temperature of the dispensed water
• T he atmospheric air pressure
• T he density of the weight used to calibrate the balance
• T his procedure can be repeated on pump 2.
Other burette sizes can be checked using the following settings:
REFERENCE
ISO/TC 48/SC1N 380E and 383E: “Piston and/or Plunger Operated
Volumetric Apparatus”
Name:
Troubleshooting 1
Method Revision:
3.0
Analysis Type:
Standard Titration
Analog Board:
Analog 1
Stirrer Configuration:
Stirrer:
Stirrer 1
Stirring Speed:
0 RPM
Pump Configuration:
Titrant Pump:
Pump 1
Reagent Addition 1:
Disabled
Reagent Addition 2:
Disabled
Dosing Type:
Linear – 20.000 mL
End Point Mode:
Fixed 10.0 mV
Pre-Titration Volume:
20.000 mL
Pre-Titration Stir Time:
0 sec
Measurement Mode:
Timed Increment
Time interval:
20 sec
Electrode Type:
Shorting Cap
Blank Option:
No Blank
Calculations:
No Formula (mL only)
Titrant Name:
DI Water
Maximum Titrant Volume:
40.000 mL
Potential Range: -2000.0 to 2000.0 mV
Volume/Flow Rate:
25 mL/50.0 mL/min
Signal Averaging:
1 Reading
Significant Figures:
XXXXX
ACCESSORIES
• H I762000C 0°C Temperature Key
• H I762070C 70°C Temperature Key
• H I70436 Deionized Water (1 gal)
• H I7662-T Temperature Probe
• S horting Cap
• N arrow Neck Beaker
• A nalytical Balance with 0.0001g resolution
DEVICE PREPARATION
• C onnect the shorting cap to the BNC socket on Analog Board 1
• Install a 25 mL burette filled with room temperature deionized
water (HI70436) on pump one and verify that no air bubbles
are present in the burette or tubing. If necessary prime the
burette until all the air has been removed completely.
• P ress
from the main screen. Use the arrow keys to
highlight HI1011EN Troubleshooting 1 and press
.
LARGE DOSE DISPENSING PROCEDURE
• Add a small amount of deionized water to a narrow neck beaker.
By doing this the air space in the beaker will be vapor-saturated
minimizing evaporation.
• P lace the narrow neck beaker on an analytical balance.
• Z ero the balance.
• Place the dosing tip through the neck of the beaker. Take care
not to immerse it in the liquid during dispensing and not to
touch the beaker walls.
• P ress
.
• Write down the exact weight displaced on the balance after
each dose.
Burette Volume
5 mL
10 mL
Pre-titration
Volume
4.000 mL
8.000 mL
TROUBLESHOOTING 1
METHOD ID: HI1011EN
Max. Titrant
Volume
8.000 mL
16.000 mL
METHOD PARAMETERS
CALCULATIONS
The measured volume of the dispensed liquid is calculated from the
measure mass using the following equation:
V
m
ρL
ρair
ρstd
Volume of measure mass of water (mL)
Measure mass of water (g)
Density of dispensed water (g/mL)
Density of ambient air (g/mL)
Density of calibration standard weight (g/mL)
21
TROUBLESHOOTING 1
METHOD ID: HI1011EN
TROUBLESHOOTING 1
ALTERNATIVE CALCULATIONS
If the actual values of the above parameters are not accessible the
following equation can be used:
V=M*F
V Volume of measured mass of water (mL)
F Transformation factor
The transformation factor takes into account the air buoyancy, the
water density and temperature dependence. Standard values can be
used to obtain the transformation factor.
The values from the table below have been calculated by correcting
the air and water density with temperature, assuming the density of
dry air ρair = 0.0012 g/mL and density of calibration steel standard
weigh ρSTD = 8 g/mL.
Temperature ( °C)
17.0
18.0
19.0
20.0
21.0
22.0
23.0
24.0
25.0
26.0
27.0
28.0
29.0
30.0
Factor
1.002290
1.002467
1.002654
1.002853
1.003061
1.003282
1.003512
1.003752
1.004002
1.004261
1.004531
1.004809
1.005097
1.005395
TEMPERATURE CHANNEL FAST CHECK PROCEDURE
• C onnect the shorting cap to the BNC socket on Analog Board 1.
• Connect the HI762000C 0°C temperature key to the RCA socket
(temperature sensor input) on Analog Board 1.
• On the main screen select
, if necessary select the
analog board and press
.
• T he titrator should display ATC 0.0 ± 0.4°C with no fluctuations
or drift.
• Connect the HI762070C 70°C temperature key to the RCA socket
(temperature sensor input) on Analog Board 1.
• The titrator should display ATC 70.0 ± 0.4°C with no
fluctuations or drift.
• T his procedure can be repeated on analog board 2.
22
TEMPERATURE & MV CHANNEL LOGGING PROCEDURE
• C onnect the shorting cap to the BNC socket on Analog Board 1.
• Connect the HI762000C 0°C temperature key to the RCA socket
(temperature sensor input) on Analog Board 1.
• On the main screen select
, if necessary select the
•
•
•
•
analog board and press
.
P ress
and use the arrow keys to highlight Logging
Interval. Set the logging interval to 15 seconds and press
. Press
to return to the main screen.
P ress the
key and use the arrow keys to highlight Setup
pH/mV/ISE Report, press
.
S elect Potential and Temperature and Units (the selected fields
are marked with an *). All other fields should be unselected.
P ress
to return to the Data Parameters screen.
• P ress
to return to the main screen.
• Once on the main screen press
to start the automatic
log.
• Let the log run for about 10 minutes. Press
to stop
the automatic log.
• P ress
, use the arrow keys to highlight Review Last
Analysis Report, and press
.
• The mV column should display 0.0 ± 0.1 mV and the
temperature column should display 0.0°C ± 0.4°C.
• This procedure can be repeated using the HI762070C 70°C
temperature key and on analog board 2.
TROUBLESHOOTING 2
DESCRIPTION
Method for verifying the dosing of the titrator. This method should be
used to troubleshoot a titrator equipped with a 25 mL burette. The
titrator dispenses a 10.00 mL pre-titration volume, waits 20 seconds
and dispenses an additional 0.5 mL dose twenty times, waiting 20
seconds between each dose, bringing the total volume to 20 mL.
This procedure can also be used to check the stirrer functionality.
The specifications of the dosing accuracy are ± 0.1% of the full
burette volume (± 0.025 mL for a 25 mL burette). For the accuracy
of other burette volumes, see the instruction manual.
If the results are not correct, check all fittings for leakage, and
burette and tubing for air bubbles. Repeat the measurement.
• T he following information is needed to verify the accuracy of the
dosing system:
• T he temperature of the dispensed water
• T he atmospheric air pressure
• T he density of the weight used to calibrate the balance
• T his procedure can be repeated on pump 2.
Other burette sizes can be checked using the following settings:
REFERENCE
ISO/TC 48/SC1N 380E and 383E: “Piston and/or Plunger Operated
Volumetric Apparatus”
METHOD PARAMETERS
ACCESSORIES
• H I762000C 0°C Temperature Key
• H I70436 Deionized Water (1 gal)
• H I7662-T Temperature Probe
• S horting Cap
• N arrow Neck Beaker
• A nalytical Balance with a resolution of 0.0001g
DEVICE PREPARATION
• C onnect the shorting cap to the BNC socket on Analog Board 1
• Install a 25 mL burette filled with room temperature deionized
water (HI70436) on pump one and verify that no air bubbles
are present in the burette or tubing. If necessary prime the
burette until all the air has been removed completely.
• P ress
from the main screen. Use the arrow keys to
highlight HI1012EN Troubleshooting 2 and press
.
SMALL DOSE DISPENSING PROCEDURE
• Add a small amount of deionized water to a narrow neck beaker.
By doing this the air space in the beaker will be vapor-saturated
minimizing evaporation.
• P lace the narrow neck beaker on an analytical balance.
• Z ero the balance.
• Place the dosing tip through the neck of the beaker. Take care
not to immerse it in the liquid during dispensing and not to
touch the beaker walls.
• P ress
.
• Write down the exact weight displaced on the balance after
each dose.
Burette Volume
5 mL
10 mL
Pre-titration
Volume
4.000 mL
8.000 mL
TROUBLESHOOTING 1
METHOD ID: HI1012EN
Max. Titrant
Volume
8.000 mL
16.000 mL
Name:
Troubleshooting 2
Method Revision:
3.0
Analysis Type:
Standard Titration
Analog Board:
Analog 1
Stirrer Configuration:
Stirrer:
Stirrer 1
Stirring Speed:
0 RPM
Pump Configuration:
Titrant Pump:
Pump 1
Reagent Addition 1:
Disabled
Reagent Addition 2:
Disabled
Dosing Type:
Linear – 0.500 mL
End Point Mode:
Fixed 10.0 mV
Pre-Titration Volume:
10.000 mL
Pre-Titration Stir Time:
0 sec
Measurement Mode:
Timed Increment
Time interval
10 sec
Electrode Type:
Shorting Cap
Blank Option:
No Blank
Calculations:
No Formula (mL only)
Titrant Name:
DI Water
Maximum Titrant Volume:
20.000 mL
Potential Range: -2000.0 to 2000.0 mV
Volume/Flow Rate:
25 mL/50.0 mL/min
Signal Averaging:
1 Reading
Significant Figures:
XXXXX
CALCULATIONS
The measured volume of the dispensed liquid is calculated from the
measure mass using the following equation:
V
m
ρL
ρair
ρstd
Volume of measure mass of water (mL)
Measure mass of water (g)
Density of dispensed water (g/mL)
Density of ambient air (g/mL)
Density of calibration standard weight (g/mL)
23
TROUBLESHOOTING 2
METHOD ID: HI1012EN
TROUBLESHOOTING 2
ALTERNATIVE CALCULATIONS
If the actual values of the above parameters are not accessible the
following equation can be used:
V=M*F
V Volume of measured mass of water (mL)
F Transformation factor
The transformation factor takes into account the air buoyancy, the
water density and temperature dependence. Standard values can be
used to obtain the transformation factor.
The values from the table below have been calculated by correcting
the air and water density with temperature, assuming the density of
dry air ρair = 0.0012 g/mL and density of calibration steel standard
weigh ρSTD = 8 g/mL.
Temperature ( °C)
17.0
18.0
19.0
20.0
21.0
22.0
23.0
24.0
25.0
26.0
27.0
28.0
29.0
30.0
24
Factor
1.002290
1.002467
1.002654
1.002853
1.003061
1.003282
1.003512
1.003752
1.004002
1.004261
1.004531
1.004809
1.005097
1.005395
STIRRING SPEED FAST CHECK PROCEDURE
• On the main screen select
, if necessary select the
•
•
•
•
•
•
analog board and press
.
P ress
and use the arrow keys to highlight Stirrer
Configuration. Use the arrow keys to highlight Stirrer 1. Press
.
Use the arrow keys to highlight Strring Speed. Use the numeric
keypad to enter 200 rpms then press
.
Press
to exit the mV Setup screen.
From the main screen, press
, use the up arrow key to
increase the stir speed slowly to 2500 rpms.
Check that the propeller continues to increase speed, following
the commands.
This procedure can be repeated on stirrer 2.
AUTOMATIC
POTENTIOMETRIC TITRATOR
TITRATION THEORY
HI932/HI931
2
TITRATION THEORY
1. GENERAL REVIEW OF TITRATION THEORY............................................................................................................. 5
1.1. INTRODUCTION TO TITRATIONS................................................................................................................................ 5
1.2.. USES OF TITRATIONS................................................................................................................................................ 5
1.3. ADVANTAGES AND DISADVANTAGES OF TITRATIONS.............................................................................................. 5
2. TYPES OF TITRATION................................................................................................................................................. 6
2.1. TITRATIONS ACCORDING TO THE MEASUREMENT METHOD..................................................................................... 6
2.1.1. AMPEROMETRIC TITRATIONS....................................................................................................................................... 6
2.1.2. POTENTIOMETRIC TITRATIONS..................................................................................................................................... 6
2.1.3. SPECTROPHOTOMETRIC TITRATIONS............................................................................................................................ 7
2.2. TITRATIONS ACCORDING TO THE REACTION TYPE................................................................................................... 8
2.2.1. ACID-BASE TITRATIONS............................................................................................................................................... 8
2.2.2. ARGENTOMETRIC TITRATIONS...................................................................................................................................... 9
2.2.3. COMPLEXOMETRIC TITRATIONS.................................................................................................................................... 9
2.2.4. ION SELECTIVE TITRATIONS......................................................................................................................................... 10
2.2.5. NON-AQUEOUS SOLVENT ACID-BASE TITRATIONS......................................................................................................... 10
2.2.6. PRECIPITATION TITRATIONS......................................................................................................................................... 11
2.2.7. REDOX TITRATIONS..................................................................................................................................................... 11
2.2.8. KARL FISCHER TITRATION............................................................................................................................................ 12
2.3. TITRATIONS ACCORDING TO THE TITRATION SEQUENCE......................................................................................... 12
2.3.1. BACK TITRATIONS....................................................................................................................................................... 12
2.3.2. MULTIPLE ENDPOINT TITRATIONS................................................................................................................................ 12
3. INTRODUCTION TO TITRATION APPARATUS AND TYPICAL TITRATION PROCEDURE..................................... 13
3.1. MANUAL TITRATION.................................................................................................................................................. 13
3.2. AUTOMATIC TITRATION.............................................................................................................................................. 13
4. TITRATION RESULTS................................................................................................................................................... 14
4.1. ACCURACY.................................................................................................................................................................. 14
4.2. REPEATABILITY.......................................................................................................................................................... 14
4.3. SOURCES OF ERROR................................................................................................................................................... 14
4.3.1. SAMPLING ERRORS..................................................................................................................................................... 14
4.3.2. ERRORS WITH TITRANT AND STANDARD....................................................................................................................... 15
4.3.2.1. PREPARATION ERRORS....................................................................................................................................... 15
4.3.2.2. DISPENSING ERRORS......................................................................................................................................... 15
4.3.3. CHEMICAL REACTION ERRORS...................................................................................................................................... 15
4.3.4. ENDPOINT DETERMINATION ERRORS........................................................................................................................... 15
5. CALCULATIONS........................................................................................................................................................... 16
5.1. SAMPLE CALCULATION.............................................................................................................................................. 16
5.2. STANDARDIZE TITRANT............................................................................................................................................. 16
5.3. BLANK TITRATION...................................................................................................................................................... 17
5.4. MULTIPLE ENDPOINT TITRATION.............................................................................................................................. 17
5.5. BACK TITRATION........................................................................................................................................................ 18
6. GLOSSARY.................................................................................................................................................................... 18
3
4
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
endpoint. This point is accompanied by an abrupt physical change in the solution, which sharply defines the endpoint of the reaction.
The physical change associated with the titration endpoint 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 is added
• The reaction must go to completion
• The reaction must have well-known stoichiometry (reaction ratios)
• A convenient endpoint 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.
TITRATION THEORY
1. GENERAL REVIEW OF TITRATION THEORY
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 foodstuffs, 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:
• 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
5
TITRATION THEORY
2. TYPES OF TITRATIONS
2.1. TITRATIONS ACCORDING TO THE MEASUREMENT METHOD
2.1.1. AMPEROMETRIC TITRATIONS
An amperometric titration is performed by placing two electrodes (often a metal ISE and a reference electrode) into the sample
solution and holding 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 endpoints. 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. 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 (silverbased) titrations.
An example of potetiometric titrations are shown below. Figure 2 “A” is the pH of a solution vs. the volume of titrant and “B” is the
potential from a chloride electrode vs. the volume of AgNO3.
6
TITRATION THEORY
Figure 2
2.1.3. SPECTROPHOTOMETRIC TITRATIONS
The name comes from the method used to detect the endpoint 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.
In the first titration curve, Figure 3 “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, Figure 3 “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 3
7
TITRATION THEORY
2.2. TITRATIONS ACCORDING TO THE REACTION TYPE
2.2.1. ACID-BASE TITRATIONS
Acid–base titrations are the most common type of titrations. They 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 endpoint 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 can be used to determine the endpoint. The indicator will change color to signify that the end of the titration
has been reached. The color of the indicator is dependent upon the concentration of ions in the solution. An acid-base indicator is
composed of a conjugate weak acid-weak base pair, where the two forms exhibit different colors depending on the pH of the solution.
For an indicator, the acid ionization constant Ka is usually written as:
HIn is the acid form of the indicator and In– is the base form. At the center of the change region, the ratio of [In–] to [HIn] is
one, [H3O+]=Ka and pH=pKa. The color change region is usually ±1 pH unit around this point. Table 1 contains a list of some
aqueous acid-base chemical indicators, as well as the pH range, the pKa and the expected color (acid and base form). When choosing
the proper indicator you should select one that has a pKa as close to the endpoint of the titration.
When chemical indicators are not suitable, a potentiometric pH titration can also be used. The pH of the solution is plotted versus the
volume of titrant added. Figure 4 shows a traditional strong acid-strong base titration curve. The graph shows the volume of NaOH
added to an acidic solution and the resulting pH of the solution. Note the abrupt change in the pH at the equivalence point.
Table 1
8
pH Range
Indicator
0.0 - 1.6
Methyl Violet
1.2 - 2.8
Thymol Blue
3.2 - 4.4
pKa
Acid Form
Base Form
Yellow
Blue
1.65
Red
Yellow
Methyl Orange
3.46
Red
Yellow
3.8 - 5.4
Bromocresol Green
4.90
Yellow
Blue
4.8 - 6.0
Methyl Red
5.00
Red
Yellow
5.2 - 6.8
Chlorophenol Blue
6.25
Yellow
Red
6.0 -7.6
Bromothymol Blue
7.30
Yellow
Blue
6.6 - 8.0
Phenol Red
8.00
Yellow
Red
7.4 -9.0
Metacresol Purple
8.30
Yellow
Purple
8.0 - 9.6
Thymol Blue
9.20
Yellow
Blue
8.2 - 10.0
Phenolphthalein
9.50
Clear
Pink
9.4 -10.6
Thymolphthalein
Clear
Blue
10.1 - 12.0
Alizarin Yellow R
Yellow
Red
11.4 - 12.6
Indigo Carmine
Blue
Yellow
TITRATION THEORY
Figure 4
2.2.2 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 (when 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 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-]).
Figure 5
2.2.3. 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.
9
TITRATION THEORY
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 endpoint 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).
Figure 6
2.2.4. 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.
2.2.5. 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.
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, dimethylformamide, 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).
10
Figure 7
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 endpoint 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.
TITRATION THEORY
TITRATION OF BASES
2.2.6. 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 then titrated with a standard solution of another reagent.
2.2.7. 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.
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.
Visual indicators such as Ferrion 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.
Figure 8
11
TITRATION THEORY
2.2.8. 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.
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 using 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.
2.3.2. MULTIPLE ENDPOINT TITRATIONS
Under certain conditions, some titrations can exhibit more than one equivalence point and be titratable to the individual endpoints
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 endpoint titrations. “A” shows the titration of a polyprotic acid. The different acid
strengths of the first and second proton can be determined. “B” illustrates a mixture of two different metal redox species, where the
different redox potentials allow the species to be separated. “C” is the titration of a solution containing strong, weak, and very weak
acids.
Figure 9
12
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 endpoint
5. The concentration of analyte is calculated based on the concentration and volume of titrant required to reach the endpoint
TITRATION THEORY
3. INTRODUCTION TO TITRATION APPARATUS AND TYPICAL TITRATION PROCEDURE
3.2. AUTOMATIC TITRATION
Automatic titrators are high-precision analytical instruments that deliver the titrant, monitor the physical change associated with the
titration reaction, automatically stop at the endpoint 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.
13
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 endpoint 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 endpoint and determine the concentration of the analyte
4. TITRATION RESULTS
4.1. ACCURACY
The factors most critical to achieving accurate results with the HI932 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, endpoint 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. ERRORS WITH TITRANT AND STANDARD
4.3.2.1. 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
14
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
TITRATION THEORY
4.3.2.2. DISPENSING ERRORS
4.3.3. 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
4.3.4. ENDPOINT DETERMINATION ERRORS
Most manual titrations use a visual indicator to indicate when the endpoint 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 (dmV vs. dV) 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 (d2 mV vs. dV2 ) 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 endpoint can result from:
• Incorrect signals from the sensor
• Sensor drift
• Sensor or instrument has slow response, keep sensors in good condition
• Inappropriate setting on the titrator
15
TITRATION THEORY
5. CALCULATIONS
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.
5.1. SAMPLE CALCULATION
By Mass
C sample
V titrant
C titrant
Ratio
FW analyte
m sample
Sample Concentration (g/100g)
Volume of titrant (L)
Titrant Concentration (eq/L)
Equivalence ratio of analyte/ titrant (mol analyte/ eq titrant)
Formula Weight of the Analyte (g/mol)
Mass of sample (g)
By Volume
C sample
V titrant
C titrant
Ratio
FW analyte
V sample
Sample Concentration (g/100mL)
Volume of titrant (L)
Titrant Concentration (eq/L)
Equivalence ratio of analyte/ titrant (mol analyte/ eq titrant)
Formula Weight of the Analyte (g/mol)
Volume of Sample (mL)
5.2. STANDARDIZE TITRANT
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 the unknown.
By Mass
C titrant
m standard
Ratio
FW standard
V titrant
16
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)
C titrant
V standard
C standard
V titrant
Concentration of titrant (N)
Volume of Standard (mL)
Concentration of standard (eq/L)
Volume of Titrant (L)
TITRATION THEORY
By Volume
5.3. 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 endpoint 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.
C Sample
C titrant
V sample
V blank
Ratio
FW analyte
m sample
Sample Concentration (g/100g)
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)
5.4. MULTIPLE ENDPOINT TITRATION
Some titrations have two or more endpoints, each corresponding to the equivalence point for a specific reaction. Multiple endpoint
titrations are similar to a blank titration in that the volume of titrant required to reach the first endpoint is subtracted from the titrant
volume used to reach the next sequential endpoint.
C sample1
C sample2
C sample3
V titrant 1
V titrant 2
V titrant 3
C titrant
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)
17
TITRATION THEORY
Ratio
FW analyte 1
FW analyte 2
FW analyte 3
m sample
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)
Weight of Sample (mL)
5.5. 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.
C sample
C titrant 1
V titrant 1
C titrant 2
V titrant 2
Ratio
FW analyte
V sample
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
A chemical species that can donate one or more protons (hydrogen ions).
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.
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
endpoint and calculate the results.
18
TITRATION THEORY
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).
Endpoint
The point were a titration is stopped because a physical change in the solution has indicated a completed titration. Titration
endpoints typically coincide with the equivalence point. A fixed value endpoint (pH or mV) can be used as well. The titration will
stop at the desired point regardless if the titration is complete.
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.
19
TITRATION THEORY
20
Manual Titration
A titration that is carried out by hand. The analyst must add the appropriate amount of titrant, determine the endpoint 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 Endpoint 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 endpoints.
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.
Non-aqueous
A solution that does not contain water.
Non-aqueous Titration
A titration that is preformed in non-aqueous solutions, typically used to titrate very weak acids and bases to eliminate the
leveling effect water has on all acids and bases dissolved in it.
Normal
The concentration of a solution which accounts for any stoichiometric difference between the various species in a solution.
Oxidation / Reduction Potential (ORP)
The measurement describing whether a species wants to donate or accept electrons from other species in a redox reaction. If a
solutions reduction potential is higher than the species it is reacting with, it will typically gain electrons or be reduced. If the
potential is lower than the species it is reacting with, it will typically lose electrons or be oxidized.
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 endpoint 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 endpoint 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.
TITRATION THEORY
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 endpoint is marked by a change in the color and/or color intensity.
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 endpoint can be
determined.
21
THEORY931/932 10/18
22
World
Headquarters
Hanna Instruments Inc.
Highland Industrial Park
584 Park East Drive
Woonsocket, RI 02895 USA
www.hannainst.com
Local Office
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Highland Industrial Park
584 Park East Drive
Woonsocket, RI 02895 USA
Phone: 800.426.6287
Fax: 401.765.7575
e-mail: tech@hannainst.com
MAN931
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