Hanna Instruments HI931 User Manual

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MANUALS

AUTOMATIC

POTENTIOMETRIC TITRATOR

HI931

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TABLE OF CONTENTS

HI931 AUTOMATIC POTENTIOMETRIC TITRATOR

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.

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QUICK START GUIDE

AUTOMATIC

POTENTIOMETRIC TITRATOR

HI931

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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.

Dear Customer,

© 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.

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INTRODUCTION .................................................................................................................................................................

SAFETY MEASURES ...........................................................................................................................................................

TITRATOR CONNECTIONS .................................................................................................................................................

USER INTERFACE ...............................................................................................................................................................

HOW TO SELECT YOUR LANGUAGE ..................................................................................................................................

HOW TO USE THE CONTEXTUAL HELP .............................................................................................................................

METHODS ..........................................................................................................................................................................

HOW TO CALIBRATE A pH ELECTRODE .............................................................................................................................

HOW TO PERFORM A TITRATION ......................................................................................................................................

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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.

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QUICK START GUIDE

TITRATOR CONNECTIONS

FRONT VIEW

REAR VIEW

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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.

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HOW TO SELECT YOUR LANGUAGE

To change the language, press from the main screen. Highlight the Language option. Using the and keys, select the language and press . Restart the titrator in order to apply the new language setting.

HOW TO USE THE CONTEXTUAL HELP

Information about the titrator can be easily accessed by pressing . The contextual help can be accessed at any time and it provides useful information about the current screen.

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.

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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 .

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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 keys to highlight a field and / to toggle the field.

• 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:

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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:

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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.

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HI931 - Titration Report

Method Name: Neutralization w/ NaOH Time & Date: 15:01 Jun 13, 2018 Report ID: Ti_00011

Calibration Data

 Buer Potential Eciency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Conguration:

Stirrer: Stirrer 1

 StirringSpeed:1400RPM

• 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).

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 PumpConguration:  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  Signicant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

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QUICK START GUIDE

 155.800193.03.614-70.525.1A00:01:31  166.07721.06.556-620.025.1A00:01:48  176.128-38.27.568-1183.225.1A00:02:03  186.177-123.69.031-1708.025.1A00:02:19  196.227-157.79.616-682.825.1A00:02:28  206.278-174.59.903-335.825.1A00:02:35  216.339-187.810.130-215.925.1A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

Page 19

INSTRUCTION MANUAL

AUTOMATIC

POTENTIOMETRIC TITRATOR

HI931

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Page 21

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.

Dear Customer,

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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

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1-1

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:

• Small footprint, requires minimal bench space

• 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.

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1-2

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2-1

SETUP

CHAPTER 2. SETUP

2.1. UNPACKING ...............................................................................................................................................................

2.2. SAFETY MEASURES ....................................................................................................................................................

2.3. INSTALLATION ...........................................................................................................................................................

2.3.1. TITRATOR FRONT VIEW ..............................................................................................................................................

2.3.2. TITRATOR REAR VIEW ................................................................................................................................................

2.3.3. TITRATOR REAR VIEW WITH PERISTALTIC PUMP ...........................................................................................................

2.3.4. TITRATOR RIGHT-SIDE VIEW .......................................................................................................................................

2.3.5. TITRATOR ASSEMBLY .................................................................................................................................................

2.3.5.1. ASSEMBLING STIRRER AND ELECTRODES HOLDER ...............................................................................................

2.3.5.2. ATTACHING STIRRER AND ELECTRODES ...............................................................................................................

2.3.5.3. CONNECTING THE PUMP ....................................................................................................................................

2.3.5.4. ATTACHING BURETTE BLANK SUPPORT ...............................................................................................................

2.3.5.5. ATTACHING THE BURETTE ..................................................................................................................................

2.3.5.6. CONNECTING PERISTALTIC PUMP TUBING ...........................................................................................................

2.3.5.7. ELECTRICAL CONNECTIONS .................................................................................................................................

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2-3

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:

ITEM 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.

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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

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SETUP

2.3.2. TITRATOR REAR VIEW

2.3.3. TITRATOR REAR VIEW WITH PERISTALTIC PUMP

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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

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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.

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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.

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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.

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SETUP

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).

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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).

Nr Function Type of Connector

Connection for pH, ORP, ISE half-cell and ISE combination electrodes

BNC Socket

B Reference electrode

4 mm Banana Socket C Temperature sensor RCA Socket D Stirrer 6-pin Connector E USB interface USB Standard B F Power input connector (24VDC) DC Power Jack Connector G External PC keyboard 6-pin Mini DIN (Standard PS2) H Printer DB-25 Socket I Extension interface 5-pin Connector J RS232 interface (Balance Interface) DB-9 Socket K Power switch

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3-1

USER INTERFACE

CHAPTER 3. USER INTERFACE

3.1. START UP...................................................................................................................................................................

3.2. DESCRIPTION ............................................................................................................................................................

3.2.1. KEYPAD ....................................................................................................................................................................

3.2.1.1. FUNCTION KEYS ................................................................................................................................................

3.2.1.2. OPTION KEYS ...................................................................................................................................................

3.2.1.3. ARROW KEYS ....................................................................................................................................................

3.2.1.4. NUMERIC KEYS .................................................................................................................................................

3.2.1.5. ENTER KEY .......................................................................................................................................................

3.2.2. DISPLAY ...................................................................................................................................................................

3.2.3. THE MAIN SCREEN.....................................................................................................................................................

3.3. MENU NAVIGATION ...................................................................................................................................................

3.3.1. SELECTING AN OPTION ...............................................................................................................................................

3.3.2. SELECTING A MENU ITEM ...........................................................................................................................................

3.3.3. ENTERING TEXT .........................................................................................................................................................

3.3.4. SAVING MODIFICATIONS ............................................................................................................................................

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USER INTERFACE

3.1. START UP

Once the instrument is assembled and installed, follow the steps below to start the titrator:

• Connect the titrator to a power outlet with the supplied power adapter.

• Turn on the titrator from the power switch located on the back of the instrument.

• Wait until the titrator finishes the initialization process.

• Press when prompted or wait a few seconds for titrator to start.

Note: All the performed initialization processes must be successfully completed. If one of the initialization processes fails, restart

the titrator. If the problem persists contact your nearest Hanna Service Center.

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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 .

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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.

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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: Displays the name of the selected method. Time and date: Displays the current date and time. Temperature reading: Displays the measured temperature.

ATC: Automatic temperature compensation Manual: Manual temperature compensation

Manual

: Temperature probe is not connected, manual temperature compensation

Stirrer information: The selected stirrer and actual/set stirrer speed is displayed in RPM. When stirrer is off, the stirrer information is not displayed. End point volume: Displays the volume delivered to reach the titration end point. When no titration

has been performed, the displayed volume is “0.000 mL”.

Result: Displays the titration result or the direct reading measurement. mV or pH reading: Displays the current readings. The reading will be in mV or pH.

mV: Indicates actual potential reading. rel mV: Indicates relative potential reading. pH: Indicates actual pH value. Titration status: Displays the status of the selected titration.

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.

No Results

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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 .

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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: To access the contextual help menu, press at any time. Help is related to the displayed screen. Press or

to return to the previous screen.

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GENERAL OPTIONS

CHAPTER 4. GENERAL OPTIONS

4.1. SAVE FILES TO USB STORAGE DEVICE ......................................................................................................................

4.2. RESTORE FILES FROM USB STORAGE DEVICE ..........................................................................................................

4.3. ADMINISTRATION .....................................................................................................................................................

4.4. TEMPERATURE ..........................................................................................................................................................

4.4.1. TEMPERATURE SOURCE .............................................................................................................................................

4.4.2. MANUAL TEMPERATURE SETTING ................................................................................................................................

4.4.3. TEMPERATURE UNITS ................................................................................................................................................

4.5. DATE AND TIME SETTING ..........................................................................................................................................

4.6. DISPLAY SETTINGS ...................................................................................................................................................

4.7. BEEPER ......................................................................................................................................................................

4.8. STIRRER .....................................................................................................................................................................

4.9. LANGUAGE ................................................................................................................................................................

4.10. TOTAL VOLUME ALERT ............................................................................................................................................

4.11. TITRANT AGE REMINDER ........................................................................................................................................

4.12. USB LINK WITH PC ..................................................................................................................................................

4.13. SETUP BALANCE INTERFACE ...................................................................................................................................

4.14. PRINTER MODE .......................................................................................................................................................

4.15. RESET TO DEFAULT SETTINGS ................................................................................................................................

4.16. OPTIMIZE MEMORY SPACE ......................................................................................................................................

4.17. UPDATE SOFTWARE ................................................................................................................................................

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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.

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4-4

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.

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The option keys allow the following operations:

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.

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.).

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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.

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4.4.1. TEMPERATURE SOURCE

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.

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.

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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 keys.

There are 8 levels of backlight intensity, ranging from 0 to 7.

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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.

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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.

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4.11. TITRANT AGE REMINDER

Option: Off, 0 to 31 days

A programmable reminder will appear when it is time to verify the titrant concentration or to change the titrant.

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.

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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 key.

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4.14. PRINTER MODE

Option: Ansi, Ascii, or Text

Ansi mode: Use 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: Use 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: This will also delete all the user - created methods and restore all manufacturer settings such as titrator configuration,

standard method parameters, etc.

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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 . When prompted, remove the USB storage and restart the titrator.

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CHAPTER 5. TITRATION METHODS

5.1. SELECTING METHODS ...............................................................................................................................................

5.2. STANDARD METHODS ...............................................................................................................................................

5.2.1. UPGRADING STANDARD METHODS ..............................................................................................................................

5.2.2. DELETING STANDARD METHODS .................................................................................................................................

5.2.3. RESTORE THE STANDARD METHODS TO THE MANUFACTURER SETTINGS ........................................................................

5.3. USER METHODS ........................................................................................................................................................

5.3.1. CREATING USER METHODS .........................................................................................................................................

5.3.2. DELETING USER METHODS .........................................................................................................................................

5.4. VIEW / MODIFY METHOD ..........................................................................................................................................

5.5. METHOD OPTIONS ....................................................................................................................................................

5.5.1. NAME .......................................................................................................................................................................

5.5.2. METHOD REVISION ....................................................................................................................................................

5.5.3. STIRRER CONFIGURATION ..........................................................................................................................................

5.5.3.1. STIRRER ...........................................................................................................................................................

5.5.3.2. STIRRER SPEED ................................................................................................................................................

5.5.4. PUMP CONFIGURATION ..............................................................................................................................................

5.5.5. DOSING TYPE ............................................................................................................................................................

5.5.5.1. LINEAR DOSING ................................................................................................................................................

5.5.5.2. DYNAMIC DOSING .............................................................................................................................................

5.5.6. END POINT MODE ......................................................................................................................................................

5.5.6.1. FIXED END POINT (pH OR mV) ...........................................................................................................................

5.5.6.2. EQUIVALENCE END POINT (pH OR mV) ...............................................................................................................

5.5.7. RECOGNITION OPTIONS (EQUIVALENCE END POINT ONLY) ............................................................................................

5.5.7.1. THRESHOLD .....................................................................................................................................................

5.5.7.2. RANGE .............................................................................................................................................................

5.5.7.3. FILTERED DERIVATIVES .....................................................................................................................................

5.5.12. PRE-TITRATION VOLUME ..........................................................................................................................................

5.5.13. PRE-TITRATION STIR TIME ........................................................................................................................................

5.5.10. MEASUREMENT MODE .............................................................................................................................................

5.5.10.1 SIGNAL STABILITY ............................................................................................................................................

5.5.10.2 TIMED INCREMENT...........................................................................................................................................

5.5.11. ELECTRODE TYPE .....................................................................................................................................................

5.5.12. BLANK OPTION ........................................................................................................................................................

5.5.13. CALCULATIONS ........................................................................................................................................................

5.5.13.1. STANDARD TITRATION .....................................................................................................................................

5.5.13.1.1. EDIT VARIABLE VALUES .............................................................................................................................

5.5.13.1.2. NO FORMULA (mL ONLY) ..........................................................................................................................

5.5.13.1.3. NO FORMULA (L ONLY) .............................................................................................................................

5.5.13.1.4. SAMPLE CALCULATION BY WEIGHT .............................................................................................................

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5.5.13.1.5. SAMPLE CALCULATION BY VOLUME ............................................................................................................

5.5.13.1.6. STANDARDIZE TITRANT BY WEIGHT ............................................................................................................

5.5.13.1.7. STANDARDIZE TITRANT BY VOLUME ...........................................................................................................

5.5.13.1.8. GENERIC FORMULA ...................................................................................................................................

5.5.14. DILUTION OPTION ...................................................................................................................................................

5.5.15. TITRANT NAME ........................................................................................................................................................

5.5.16. TITRANT CONCENTRATION ........................................................................................................................................

5.5.17. ANALYTE SIZE ..........................................................................................................................................................

5.5.18. ANALYTE ENTRY .......................................................................................................................................................

5.5.18.1. FIXED WEIGHT OR VOLUME .............................................................................................................................

5.5.18.2. MANUAL WEIGHT OR VOLUME .........................................................................................................................

5.5.19. MAXIMUM TITRANT VOLUME ....................................................................................................................................

5.5.20. POTENTIAL RANGE ...................................................................................................................................................

5.5.21. VOLUME/FLOW RATE ...............................................................................................................................................

5.5.22. SIGNAL AVERAGING .................................................................................................................................................

5.5.23. SIGNIFICANT FIGURES .............................................................................................................................................

5.6. PRINTING ..................................................................................................................................................................

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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.

5.1. SELECTING METHODS

To select a method, press from the main screen. A list of available methods will be displayed.

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.

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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 or keys to remove unnecessary standard methods.

• Press to return to the General Options screen.

From PC:

Unnecessary standard methods can be removed from the titrator using the HI900 PC application (see General Options section).

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 .

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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.

5.3. USER METHODS

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 from the main screen.

• Using the and keys, highlight an existing method from the method list.

• Press . A new user method will be generated.

• Press to activate the new user method.

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5.5. METHOD OPTIONS

Note: Only certain method options can be changed for standard methods.

5.5.1. NAME

Option: Up to 24 characters

5.4. 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.

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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

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5.5.3.2. STIRRER SPEED

Option: 200 to 2500 RPM

5.5.4. PUMP CONFIGURATION

Option: Pump 1 or Pump 2 (if installed)

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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

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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.

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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.

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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

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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.

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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).

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5.5.7. RECOGNITION OPTIONS (EQUIVALENCE END POINT ONLY)

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.

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.

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Depending on the titration curve profile, the following guide can be used:

TITRATION CURVE PROFILE THRESHOLD (mV/mL)

Flat 1 to 450

Normal 50 to 1800

Steep 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.

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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.

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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.

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5.5.10. MEASUREMENT MODE

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.

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.

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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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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).

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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.

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5.5.13.1.4. SAMPLE CALCULATIONS BY WEIGHT

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.

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/L grams/liter mg/L milligrams/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/g milligrams/gram mg/kg milligrams/kilogram mol/kg moles/kilogram mmol/g millimoles/gram eq/kg equivalents/kilogram meq/kg milliequivalents/kilogram

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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/L grams/liter mg/L milligrams/liter

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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/L milligrams/liter µg/L micrograms/liter mmol/L millimoles/liter mg/mL milligrams/milliliter mg/100 mL milligrams/100 milliliters g/100 mL grams/100 milliliters eq/L equivalents/liter meq/L milliequivalents/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:

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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:

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5.5.13.1.8. GENERIC FORMULA

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.

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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 moles/Liter eq/L equivalents/Liter g/L grams/Liter mg/L 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 H2SO

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

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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.

Final Dilution Volume: The volume of the sample after dilution Aliquot Volume: Volume of sample taken from the dilution for titration Analyte size to be diluted: The initial sample weight (volume)

5.5.15. TITRANT NAME

Option: Up to 15 characters

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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

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5.5.18.1. FIXED WEIGHT OR VOLUME

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

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.

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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.

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5.5.23. SIGNIFICANT FIGURES

Option: Two (XX), Three (XXX), Four (XXXX) or Five (XXXXX)

This option allows you to set the format for displaying the final titration result.

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).

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TITRATION MODE

CHAPTER 6. TITRATION MODE

6.1. RUNNING A TITRATION.............................................................................................................................................

6.1.1. STARTING A TITRATION ..............................................................................................................................................

6.1.2. SUSPENDING A TITRATION .........................................................................................................................................

6.1.3. VIEWING THE TITRATION CURVE .................................................................................................................................

6.2. STOPPING A TITRATION ...........................................................................................................................................

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6.1. RUNNING A TITRATION

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.

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 . This will stop the dosing pump if it is running. To continue the titration press .

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”.

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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).

- 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.

Figure 1

Figure 3

Figure 2

Figure 4

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6.2. STOPPING A TITRATION

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.

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pH MODE

CHAPTER 7. pH MODE

7.1. DISPLAY.....................................................................................................................................................................

7.2. pH SETUP ..................................................................................................................................................................

7.2.1. BUFFER ENTRY TYPE ..................................................................................................................................................

7.2.2. FIRST CALIBRATION POINT .........................................................................................................................................

7.2.3. EDIT CUSTOM BUFFERS .............................................................................................................................................

7.2.4. EDIT BUFFER GROUP .................................................................................................................................................

7.2.5. CALIBRATION REMINDER ............................................................................................................................................

7.2.6. SET REMINDER PERIOD ..............................................................................................................................................

7.2.7. CLEAR CALIBRATION...................................................................................................................................................

7.2.8. pH GLP DATA .............................................................................................................................................................

7.2.9. LOGGING INTERVAL ....................................................................................................................................................

7.2.10. STABILITY CRITERIA .................................................................................................................................................

7.2.11. pH RESOLUTION ......................................................................................................................................................

7.2.12. STIRRER CONFIGURATION ........................................................................................................................................

7.2.13. STIRRING SPEED .....................................................................................................................................................

7.3. pH CALIBRATION .......................................................................................................................................................

7.4. LOGGING ...................................................................................................................................................................

7.4.1. INTERVAL LOGGING ....................................................................................................................................................

7.4.2. MANUAL LOGGING .....................................................................................................................................................

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Hanna Instruments HI931 User Manual

Specifications and Main Features

Frequently Asked Questions

User Manual