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A2-1

APPENDIX 2

Appendix 2. Back Titration

BACK TITRATION

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A2-3

A2.1 Applicability Domain

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A2-3

A2.2 Method Principles

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A2-3

A2.3 Example of a Back Titration

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A2-3

A2.3.1 Introduction ........................................................................................... A 2 - 3

A2.3.2 Setting Up the Method Parameters ............................................................ A 2 - 4

A2.3.3 Preparing the Sample .............................................................................. A 2 - 5

A2.3.4 Perform the Titration ............................................................................... A 2 - 5

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Summary of Contents for HI 902 Color

Page 1: ...1 QUICK START GUIDE HI 902 Color AUTOMATIC POTENTIOMETRIC TITRATOR Revision 2 00 sale ponpe com www ponpe com ...

Page 2: ...essary information for the correct use of the instrument The purpose of this guide is to present a quick overview of setting up and using the instrument For detailed information illustrating the extensive capabilities of your titrator please refer to the Instruction Manual 2010 Hanna Instruments All rights are reserved Reproduction in whole or in part is prohibited without the written consent of t...

Page 3: ...ODUCTION 4 SAFETY MEASURES 5 TITRATOR CONNECTIONS 6 USER INTERFACE 7 HOW TO SELECT YOUR LANGUAGE 8 HOW TO USE THE CONTEXTUAL HELP 8 METHODS 8 HOW TO CALIBRATE A pH ELECTRODE 9 HOW TO PERFORM A TITRATION 10 sale ponpe com www ponpe com ...

Page 4: ...via a USB interface saved to a USB storage device or printed directly from the titrator An external monitor and 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 interfac...

Page 5: ...ed tubing are assembled correctly 4 Always check that the titrant bottle and the titration beaker are placed on a flat stable surface 5 Always wipe up spills and splashes immediately 6 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 7 Hav...

Page 6: ...6 QUICK START GUIDE TITRATOR CONNECTIONS Front View Rear View sale ponpe com www ponpe com ...

Page 7: ...lit display The main screen is shown below with short explanations The user interface contains several screens In each screen many information fields are present at the same time The information is displayed in an easy to read manner Virtual option keys describe the function performed when the corresponding option key is pressed sale ponpe com www ponpe com ...

Page 8: ...ntextual help can be accessed at any time and it provides useful information about the current screen METHODS The HI 902 titrator can store up to 100 methods Standard Methods Each titrator is supplied with a package of standard methods Standard method packs are developed at Hanna Instruments laboratories to meet analysis requirements of specific industries e g water treatment wine dairy etc User D...

Page 9: ...ared the old calibration can be cleared by pressing Note It is very important to clear calibration history when a new electrode is used because most errors and warning messages that appear during calibration depend on calibration history 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 Im...

Page 10: ...te 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 F...

Page 11: ...hen press Highlight Analyte Size option then press Enter the volume of the sample ex 5 mL then press Press highlight Save Method option and then press 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 dis played Highlight Setup Titration Rep...

Page 12: ... 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 Note Make sure that the pH electrode temperature probe and propeller do not touch each other or the beaker 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 st...

Page 13: ... 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 When the titration has ended the titrator will display the equivalence endpoint volume and the final concentrati...

Page 14: ...e 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 sessi...

Page 15: ...ffer Potential Efficiency Temperature Time and Date 4 006pH 169 9mV 100 7 A 22 00 C 10 20 Apr 16 2010 7 020pH 7 8mV 96 5 A 22 00 C 10 23 Apr 16 2010 10 040pH 178 6mV 96 5 A 21 90 C 10 25 Apr 16 2010 GLP Instrumentation Data Sample Name Sample HCl 1 Company Name Hanna Instruments Operator Name Electrode Name HI 1131 NO 2 Field 1 Any text Field 2 Any text Field 3 Any text Titrator Software Version v...

Page 16: ...0 RPM Potential Range 2000 0 to 2000 0 mV Volume Flow Rate 25 mL 50 0 mL min Signal Averaging 1 Reading Final Result Format X XX M mol L M mol L V mol mol L mol mL L 1000mL V volume dispensed in liters 0 100 mol L titrant conc 1 000 mol mol sample titrant 5 000 mL sample volume Nr Volume ml mV pH Graphic Temp 0 C Time 0 0 000 235 2 2 857 0 0 A 1 9 1 0 0 0 0 0 0 1 0 050 234 6 2 866 10 2 A 1 9 0 0 0...

Page 17: ... 3 30 4 889 153 7 4 253 189 9 A 1 9 2 0 0 0 3 5 4 31 4 915 147 1 4 367 259 9 A 1 9 2 0 0 0 4 0 0 32 4 934 141 0 4 471 322 7 A 1 9 2 0 0 0 4 1 1 33 4 949 135 2 4 571 388 0 A 1 9 2 0 0 0 4 1 7 34 4 964 127 5 4 702 512 0 A 1 9 2 0 0 0 4 2 3 35 4 979 117 3 4 877 680 0 A 1 9 2 0 0 0 4 2 9 36 4 994 104 2 5 102 875 3 A 1 9 2 0 0 0 4 3 5 37 5 009 87 9 5 381 1088 0 A 1 9 2 0 0 0 4 4 1 38 5 024 69 6 5 695 1...

Page 18: ...18 QUICK START GUIDE QS 902C 10 10 sale ponpe com www ponpe com ...

Page 19: ...1 INSTRUCTION MANUAL HI 902 Color AUTOMATIC POTENTIOMETRIC TITRATOR Revision 2 00 www ponpe com sale ponpe com ...

Page 20: ... correct use of the instrument This instruction manual has been written for the HI 902 titrators with color display USB interface and software version 2 00 or later 2010 Hanna Instruments All rights are reserved Reproduction in whole or in part is prohibited without the written consent of the copyright owner Hanna Instruments Inc 584 Park East Drive Woonsocket Rhode Island 02895 USA sale ponpe com...

Page 21: ...hapter 5 METHODS Chapter 6 TITRATION MODE Chapter 7 pH mV and ISE MODE Chapter 8 AUXILIARY FUNCTIONS Chapter 9 MAINTENANCE PERIPHERALS Appendix 1 TECHNICAL SPECIFICATIONS Appendix 2 BACK TITRATION Appendix 3 MULTIPLE EQUIVALENCE POINTS Appendix 4 LINKED METHOD Appendix 5 ACCESSORIES sale ponpe com www ponpe com ...

Page 22: ...1 2 INTRODUCTION sale ponpe com www ponpe com ...

Page 23: ... LCD in the selected units Titration graph can be displayed on the LCD and saved as a bitmap Customizable titration reports can be printed saved on a USB storage device or transferred to a PC via the USB interface Direct measurements The titrator can also be used as a mV pH or ISE meter Data logging is available for mV pH and ISE measurements GLP features Up to 5 calibration points Reminders for t...

Page 24: ...1 2 INTRODUCTION sale ponpe com www ponpe com ...

Page 25: ... Titrator Rear View 2 5 2 3 3 Titrator Left side View 2 6 2 3 4 Titrator Assembly 2 6 2 3 4 1 Assembling Stirrer Stand and Support 2 6 2 3 4 2 Attaching Stirrer 2 7 2 3 4 3 Connecting the Pump 2 8 2 3 4 4 Attaching Burette Blank Support 2 8 2 3 4 5 Attaching the Burette 2 9 2 3 4 6 Electrical Connections 2 1 0 sale ponpe com www ponpe com ...

Page 26: ...2 2 SETUP sale ponpe com www ponpe com ...

Page 27: ...lar and positioning screw 5 Burette Blank Support 1 pcs 6 Pump and Burette Locking Screws with Plastic Head 2 pcs 7 Temperature Sensor 1 pcs 8 Shorting Cap 1 pcs 9 Power Cable 1 pcs 10 USB Cable 1 pcs 11 Instruction Manual Binder 1 pcs 12 USB Memory Stick 1 pcs 13 HI 900 PC Application Installation Kit on USB Stick 1 pcs 14 Quality Certificate 1 pcs See Appendix 4 section A 4 3 Titrator components...

Page 28: ... correctly see Section 9 1 Burette Maintenance for more details 4 Always check that the titrant bottle and the titration beaker are on a flat surface 5 Always wipe up spills and splashes immediately 6 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 Explosi...

Page 29: ...2 5 SETUP 2 3 Installation 2 3 1 Titrator Front View 2 3 2 Titrator Rear View www ponpe com sale ponpe com ...

Page 30: ...to the power supply 2 3 4 1 Assembling Stirrer Stand and Support To assemble the stirrer stand and support Remove the screws B from the titrator base A Attach the stirrer stand C to the titrator Tighten the stirrer stand C using the previously removed screws B Screw the stirrer support D in the stirrer stand C sale ponpe com www ponpe com ...

Page 31: ...rer A by pressing it onto the stirrer shaft Insert the electrode C and temperature sensor D into the dedicated holes on the stirrer Push them in until they are in a stable position Slide the stirrer on the stirrer support and set the height by tightening the screw located on the positioning collar E sale ponpe com www ponpe com ...

Page 32: ...e it towards the front of the titrator chassis C until it is firmly latched Secure the pump with the locking screw D This procedure can be repeated to connect a second pump 2 3 4 4 Attaching Burette Blank Support To attach the burette blank support follow these steps Insert burette blank support in to the bay Lower the burette blank support into the titrator then slide it towards the front of the ...

Page 33: ...ing cap and from the burette body are aligned as shown in Figure 2 While ensuring the correct coupling between the syringe plunge 1 and the pump piston 2 Figure 3 slide the burette into the support on the burette pump Figure 4 Figure 2 Figure 3 Figure 4 sale ponpe com www ponpe com ...

Page 34: ... IEC Power Line Connector Check on titrator rear panel M C Temperature sensor RCA Socket D Stirrer 4 pin Mini DIN E RS232 interface Balance Interface Standard DB 9 Pin Socket F Connector for expansion device 8 pin Mini DIN G External PC keyboard 6 pin Mini DIN Standard PS2 H External display Standard VGA Display 15 pin Socket I Printer DB 25 pin Socket J USB interface USB Standard B K Connection f...

Page 35: ...unction Keys 3 4 3 2 1 2 Option Keys 3 4 3 2 1 3 Arrow Keys 3 5 3 2 1 4 Numeric Keys 3 5 3 2 1 5 Enter Key 3 5 3 2 2 Display 3 5 3 2 3 The Main Screen 3 6 3 3 Menu Navigation 3 7 3 3 1 Selecting an Option 3 7 3 3 2 Selecting a Menu Item 3 7 3 3 3 Entering Text 3 7 3 3 4 Saving Modifications 3 8 sale ponpe com www ponpe com ...

Page 36: ...3 2 USER INTERFACE sale ponpe com www ponpe com ...

Page 37: ...fied by the titrator 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 them is terminated by a Failed message restart the titrator from the power switch If ...

Page 38: ...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 stirrer ON and OFF Reserved Access the results menu 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...

Page 39: ...c Keys Keys to Used for numeric entries Toggles between positive and negative values Decimal point Initiates entry of exponent for scientific notation 3 2 1 5 Enter Key Both keys perform the same 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 explana...

Page 40: ...M 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 Titration result Displays the titration result mV or pH reading Displays the current readings The reading will be in mV or pH mV Indicates actual potential reading rel mV Indicates relati...

Page 41: ...r 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 T...

Page 42: ...een 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 press again to return to the previous screen sale ponpe com www ponpe com ...

Page 43: ...ng 4 5 4 3 Display Settings 4 6 4 4 Beeper 4 7 4 5 Stirrer 4 7 4 6 Language 4 8 4 7 Total Volume Alert 4 8 4 8 Titrant Age Reminder 4 9 4 9 Save Files to USB Storage Device 4 9 4 10 Restore Files from USB Storage Device 4 10 4 11 USB Link with PC 4 11 4 12 Setup Balance Interface 4 12 4 13 Printer Mode 4 13 4 14 Reset to Default Settings 4 13 4 15 Update Software 4 14 sale ponpe com www ponpe com ...

Page 44: ...4 2 GENERAL OPTIONS sale ponpe com www ponpe com ...

Page 45: ...at are not directly related to the titration process or pH mV ISE measurement To access this screen press from the main screen The available menus are described below 4 1 Temperature The Temperature Menu allows access to all of the settings related to temperature sale ponpe com www ponpe com ...

Page 46: ...creen 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 1 2 Manual Temperature Setting If the temperature probe is not connected the user can manually set the temperature used by the titrator for compensation This can be done when the Manual Temperature option is selected...

Page 47: ...ime 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 1 3 Temperature Units The following temperature units can be selected sale ponpe com www ponpe com ...

Page 48: ...ropriate 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 i...

Page 49: ...rn the Beeper On Enable or Off Disable The beeper will sound after a titration is completed when an invalid key is pressed or when a critical error occurs during titration 4 5 Stirrer This screen allows the stirrer to be enabled or disabled sale ponpe com www ponpe com ...

Page 50: ...ume will decrease as the titrant is used The Low Titrant Volume reminder message will appear when the available titrant volume is under 100 mL After the new titrant volume has been set on the titrator in the Total Volume Alert screen a warning message appears reminding the user to perform titrant re standardization The volume of titrant can be set from 0 to 10 000 mL sale ponpe com www ponpe com ...

Page 51: ... to 31 days 4 9 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 p...

Page 52: ...o the General Options screen The status of the transfer successful unsuccessful and the file name of the currently pro cessed file are displayed during copying or deleting Note The saved files will be stored on the USB key in the HI902 folder as follows Methods USB Drive HI902 Methods mtd Reports USB Drive HI902 Reports rpt 4 10 Restore Files from USB Storage Device This screen allows the user to ...

Page 53: ...yed files from diskette to the USB storage device Returns to the General Options screen Note In order to restore files from USB key please ensure that the methods and or reports you wish to transfer to the titrator are in the correct folder Methods USB Drive HI902 Methods mtd Reports USB Drive HI902 Reports rpt 4 11 USB Link with PC In order to use this feature the USB cable needs to be connected ...

Page 54: ...utomatic weight acquisition will be not available Press to customize the serial communication parameters by accessing the Balance Configuration screen Be sure that the settings on the titrator Balance Configuration menu match the settings for your particular balance baud rate data bits parity stop bit number request command syntax It may be necessary to change settings on your balance Users should...

Page 55: ... 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 14 Reset to Default Settings This option restores the manufacturer settings Note Please be careful This will also delete all the user created methods and restore all man...

Page 56: ...4 14 GENERAL OPTIONS 4 15 Update Software This screen allows the user to update the titrator software from a USB storage device containing a software setup kit sale ponpe com www ponpe com ...

Page 57: ...ethod Options 5 7 5 5 1 Naming the User Method 5 7 5 5 2 Method Revision 5 8 5 5 3 Titration Type 5 8 5 5 4 Pump Configuration 5 9 5 5 5 Dosing Type 5 10 5 5 5 1 Linear Dosing 5 10 5 5 5 2 Dynamic Dosing 5 11 5 5 6 End Point Mode 5 13 5 5 6 1 Fixed End Point pH or mV 5 13 5 5 6 2 Equivalence End Point pH or mV 5 14 5 5 7 Recognition Options Equivalence End Point pH or mV only 5 17 5 5 7 1 Threshol...

Page 58: ...ight 5 33 5 5 13 8 2 Sample Calculation by Volume 5 35 5 5 13 8 3 Generic Formula 5 37 5 5 14 Dilution Option 5 37 5 5 15 Titrant Name 5 38 5 5 16 Titrant Concentration 5 38 5 5 17 Analyte Size 5 38 5 5 18 Analyte Entry 5 38 5 5 18 1 Fixed Weight or Volume 5 39 5 5 18 2 Manual Weight or Volume 5 39 5 5 18 3 Same as Previous Linked Methods only 5 39 5 5 19 Titrant 1 Entry Back Titration only 5 39 5...

Page 59: ... a pack of standard 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 To select a method highlight the method and press The name of the selected method will be displayed on the ma...

Page 60: ...hods 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 HI 900 PC applica tion see section 4 13 USB Link with PC 5 2 2 Deleting Standard Methods Unnecessary standard methods can be removed from the titrator by following the procedure below From ...

Page 61: ...tandard 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 methods list Press A new user method will be generate...

Page 62: ...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 4 View Modify Method To modify the method s 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 mo...

Page 63: ... name for the new method up to 24 characters Use the arrow keys to navigate through the character table Press to add the highlighted character to the method name To exit the View Modify Method screen press You can choose to save the modifications or to discard them sale ponpe com www ponpe com ...

Page 64: ...mple is consumed by a known volume and concentration of titrant 1 A sufficient amount of titrant 1 is dispensed to surpass the equivalence point in order to react quickly with the sample Phase 2 the excess of titrant 1 is titrated with the titrant 2 to the equivalence point The concentration of the sample is determined by the amount of titrant used in phase 2 5 5 2 Method Revision This option allo...

Page 65: ...hase of the back titration A break in the titrant will allow you to perform a task related to the analysis e g boiling the sample to remove carbon dioxide 5 5 4 Pump Configuration This option allows you to choose the pump that will be used for the titration For a Back Titration you can select the pump to be used for titrant 1 and titrant 2 sale ponpe com www ponpe com ...

Page 66: ...ements are recommended to obtain many measured points around the equivalence point For flat titration curves larger volume increments are recommended for equivalence point detection Linear Dosing 5 5 5 Dosing Type The Titrator has two dosing types Linear Dosing and Dynamic Dosing 5 5 5 1 Linear Dosing Linear dosing dispenses a pre defined volume of titrant with every addition see graph sale ponpe ...

Page 67: ...wer 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 the 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 t...

Page 68: ...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 t...

Page 69: ...ration 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 The range is from 2 000 to 20 000 pH sale ponpe com www ponpe com ...

Page 70: ... value is expressed in mV The range is from 2000 0 to 2000 0 mV 5 5 6 2 Equivalence End Point pH or mV The titration is normally terminated when the equivalence point is detected the point where the added quantity of titrant equals the quantity of analyte present in the sample sale ponpe com www ponpe com ...

Page 71: ...alence point is reached The reported end point volume is a calculated value based on a number of points around the equivalence point The potentiometric S shaped titration curve is the response in potential mV or pH between the indication of the electrode versus the volume of titrant added The inflection point of the S shaped titration curve is assumed to be the equivalence point of the chemical re...

Page 72: ...e 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 on page 5 17 sale ponpe com www ponpe com ...

Page 73: ... first derivative must be greater than the threshold value see Recogni tion Options on page 5 17 5 5 7 Recognition Options Equivalence End Point pH or mV 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 concentra tions and or electrode response The Recognition Options screen is av...

Page 74: ...mL below which the detection algorithm does not search for the equivalence point Range is between 1 and 9999 mV mL The recommended value is 40 of the absolute value of the first derivative 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 sale ponpe com www ponpe com ...

Page 75: ... 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 pH Range 2 000 to 20 000 mV Range 2000 0 to 2000 0 The Limit 2 value must not be equal to the Limit 1 value sale ponpe com www ponpe com ...

Page 76: ...gnal Stability Stirring Speed etc Insufficient titrant additions Note A shift in the endpoint volume by 1 or 2 doses may be seen due to filtering 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 direct...

Page 77: ... considerably shorten the overall titration duration 5 5 9 Pre Titration Stir Time 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 range is from 0 to 180 seconds The Pre Titration Stir Time option is disabled if 0 seconds is entered sale ponpe com www ponpe com ...

Page 78: ...y 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...

Page 79: ...l is measured The range is from 0 5 to 10 0 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 fr...

Page 80: ... 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 The range is from 2 to 180 seconds sale ponpe com www ponpe com ...

Page 81: ...ect 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 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 sale ponpe com www ponpe com ...

Page 82: ...ption allows the user to edit the variables in a previously selected calculation For each formula selected variables can be changed 5 5 13 1 No Formula mL only If this option is selected only the volume of titrant mL required to reach the end point is displayed 5 5 13 2 No Formula L only If this option is selected only the volume of titrant L required to reach the end point is displayed sale ponpe...

Page 83: ...nits 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 milli...

Page 84: ...on 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 When choosing the formula select the Titrant Unit first and then the Final Sample Unit 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 mill...

Page 85: ... 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 equivalences liter meq L milliequivalences liter A formula example is shown below using N eq L as the titrant units and ppt g L as the final result units Variables can be set according to the amount of sample and titrant used sale...

Page 86: ...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 titrator will perform the calculation based on the titrant unit selected The calculation is based on the selected titrant unit If the titrant unit is N eq L the formula ...

Page 87: ...gram N eq L Normality equivalents liter mg kg milligrams kilogram mg L milligrams liter mol kg moles kilogram µg L micrograms 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 re...

Page 88: ...ram 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...

Page 89: ...5 33 METHODS 5 5 13 8 Back Titrations 5 5 13 8 1 Sample Calculations by Weight Select the titrant 1 unit the titrant 2 unit and the final result unit sale ponpe com www ponpe com ...

Page 90: ...1 needed to consume the sample and multiply it with the excess factor in order to raise or lower the amount of titrant 1 dispensed Variables can be set according to the amount of sample and titrant used Press to proceed to the next formula If you do not want the titrator to calculate the volume of titrant 1 to add see Section 5 5 18 Titrant 1 Entry The remaining volume of titrant 1 needs to be cal...

Page 91: ... the variables are set press to proceed with the Calculating Sample Concentration formula 5 5 13 8 2 Sample Calculations by Volume Select the titrant 1 unit titrant 2 unit and the final result unit sale ponpe com www ponpe com ...

Page 92: ...or will calculate the volume of titrant 1 needed to consume the sample and multiply it with the excess factor in order to raise or lower the amount of titrant 1 dispensed Variables can be set according to the amount of sample and titrant used Press to proceed to the next formula If you do not want the titrator to calculate the volume of titrant 1 to add see Section 5 5 18 Titrant Entry The followi...

Page 93: ...on in a solid or liquid sample 5 5 14 Dilution Option 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 Sample volume used for ...

Page 94: ...eport 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 The titrant concentration can not be set 5 5 17 Analyte Size Enter the size of the sample for sample concentration determinations or standard for titrant concentration determination 5 5 18 Analyte Entry Select the analyte entry mod...

Page 95: ...The same weight or volume is used for both methods 5 5 19 Titrant 1 Entry Back Titration Only Select the mode for evaluating the necessary quantity of titrant 1 used in the back titration process phase 1 5 5 19 1 Calculated by Formula The volume of titrant 1 to be dispensed in the phase 1 of back titration will be calculated by the titrator see section 5 5 12 2 Back Titrations 5 5 19 2 Fixed by Us...

Page 96: ...ed after the maximum titrant volume has been dispensed The error message Lim its Exceeded will appear on the display Range is from 0 100 to 100 000 mL 5 5 21 Stirring Speed The stirring speed can be set between 100 and 2500 RPM with 100 RPM resolution The stir speed from the current method is used during the entire titration The speed can be adjusted at any time using the and keys when the stirrer...

Page 97: ...ntial over range The ranges can be set between 2000 0 to 2000 0 mV 5 5 23 Volume Flow Rate The flow rate for the dosing system can be set by the user in an interval of 0 1 to two times the burette volume 0 1 to 10 mL min for a 5 mL burette 0 1 to 20 mL min for a 10 mL burette 0 1 to 50 mL min for a 25 mL burette Note The titrator will automatically detect the burette size and display the correct h...

Page 98: ... it into a moving window along with the last 2 3 or 4 readings depending on the selected option The average of those readings is displayed and used for calculations Averaging more readings is helpful when a noisy signal is received from the electrode 5 5 25 Final Result Format This option allows you to set the format for displaying the final titration result sale ponpe com www ponpe com ...

Page 99: ... offline an error message will appear on the display see 9 3 3 Connecting a Printer section for information about connecting a printer to the titrator 5 5 26 Linked Method This option allows the user to link two titration methods If No Link is selected only the current method will run If a method is selected it will run after the current method See Appendix 4 for additional information sale ponpe ...

Page 100: ...5 44 METHODS sale ponpe com www ponpe com ...

Page 101: ...pter 6 Contents 6 TITRATION MODE 6 3 6 1 Running a Titration 6 3 6 1 1 Starting a Titration 6 3 6 1 2 Suspending a Titration 6 3 6 1 3 Viewing the Titration Curve 6 3 6 2 Stopping a Titration 6 5 sale ponpe com www ponpe com ...

Page 102: ...6 2 TITRATION MODE sale ponpe com www ponpe com ...

Page 103: ...ns The stirrer will turn on if detected and enabled If the pre stirring time option is enabled the sample will be stirred until the set time elapses see section 5 5 9 Pre Titration Stir Time If the pre titration volume option is enabled the set volume will be dispensed see section 5 5 8 Pre Titration Volume The titrator will start the analysis and continue to deliver titrant until the end point is...

Page 104: ...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 only the mV vs volume curve is display...

Page 105: ... The endpoint was successfully detected The final results will be displayed Manually Terminated The current titration terminated by the user before the endpoint was detected Limits Exceeded The maximum titrant volume was delivered without reaching the endpoint An error message is displayed on the screen Critical Error A critical error occurred and the titration was stopped These errors are typical...

Page 106: ...6 6 TITRATION MODE sale ponpe com www ponpe com ...

Page 107: ...10 Stability Criteria 7 10 7 1 2 11 pH Resolution 7 11 7 1 2 12 Stirrer Configuration 7 11 7 1 2 13 Stirring Speed 7 12 7 1 3 pH Calibration 7 12 7 2 mV Mode 7 15 7 2 1 Display 7 15 7 2 2 mV Setup 7 15 7 2 2 1 Clear Relative mV Offset 7 16 7 2 2 2 Logging Interval 7 16 7 2 2 3 Stability Criteria 7 17 7 2 2 4 Stirrer Configuration 7 17 7 2 2 5 Stirring Speed 7 18 7 2 3 mV Rel Calibration 7 18 7 3 I...

Page 108: ...4 7 3 2 9 ISE GLP Data 7 24 7 3 2 10 Electrode Type 7 25 7 3 2 11 Concentration Unit 7 26 7 3 2 12 Logging Interval 7 26 7 3 2 13 Stability Criteria 7 27 7 3 2 14 ISE Significant Digits 7 27 7 3 2 15 Stirrer Configuration 7 28 7 3 2 16 Stirring Speed 7 28 7 3 3 ISE Calibration 7 28 7 4 Logging 7 30 7 4 1 Automatic Logging 7 3 0 7 4 2 Manual Logging 7 3 0 sale ponpe com www ponpe com ...

Page 109: ...or ISE modes One Analog Board Switches to Titrator mode Switches to pH mode Switches to mV mode Switches to ISE mode Two Analog Boards Switches to Titrator mode or Switches the Analog Input for pH mV and ISE mode Switches to pH mode Switches to mV mode Switches to ISE mode pH mV ISE MODE sale ponpe com www ponpe com ...

Page 110: ...l Options for more information Stores the current pH reading see section 7 4 2 Manual Logging or Starts the pH automatic log see section 7 4 1 Automatic Logging Enter the pH calibration screen see section 7 1 3 pH Calibration Enter the pH setup screen parameters are associated with pH measurements and calibration see section 7 1 2 pH Setup Allow the user to switch between the available measurement...

Page 111: ...tomatic the instrument automatically selects the pH calibration point as the closest buffer from the predefined Buffer Group see section 7 1 2 4 Edit Buffer Group Semiautomatic the instrument automatically selects the closest buffer from Available Buffers standard and custom buffers Manual the calibration buffer must be manually selected by the user during calibration from the available buffer lis...

Page 112: ...ded perform a one point calibration using the Offset option The existing slope values will not be changed 7 1 2 3 Edit Custom Buffers If you wish to use buffers other than the standard ones the Edit Custom Buffers option is available allowing you to set the desired pH buffers Up to five pH custom buffers can be set Note Custom buffers are not temperature compensated The value of the buffer at the ...

Page 113: ...e buffers Hanna or Custom to be used for automatic buffer recognition Automatic Buffer Entry Type Within the Buffer Group pH values must be at least 1 5 pH far apart If the Buffer Group already contains five pH buffers at least one pH buffer has to be removed in order to add another buffer Use the arrow keys to select the pH buffer to be included removed in from the buffer group Press or to add re...

Page 114: ...eriodic the calibration reminder will appear after the set time has elapsed since the last calibration Disable the calibration reminder will not appear 7 1 2 6 Set Reminder Period If Daily or Periodic option was selected for the Calibration Reminder the reminder period must also be set For a daily reminder period the time of day can be set For a periodic reminder period the number of days hours an...

Page 115: ...urn to pH setup 7 1 2 7 Clear Calibration This option clears the existing pH calibration for the selected channel If the calibration is cleared another calibration has to be performed Press to clear the previous calibration or to return to the previous screen without clearing the calibration 7 1 2 8 pH GLP Data Displays the pH calibration data sale ponpe com www ponpe com ...

Page 116: ...terval to be used for automatic logging 7 1 2 10 Stability Criteria Select the signal stability criteria Fast quicker results with less accuracy Medium medium speed results with medium accuracy Accurate slower results with high accuracy sale ponpe com www ponpe com ...

Page 117: ...DE 7 1 2 11 pH Resolution Set the desired pH resolution one x x two x xx or three x xxx decimals 7 1 2 12 Stirrer Configuration Set the stirrer configuration Stirrer 1 Stirrer 2 or Disabled sale ponpe com www ponpe com ...

Page 118: ...s When No pH Calibration or pH Calibration Expired message appears on the LCD in the Reminder messages area PREPARATION Pour small quantities of the buffer solutions into clean beakers If possible use plastic beakers to minimize any EMC interferences For accurate calibration and to minimize cross contamination use two beakers for each 7 1 2 13 Stirring Speed The stirring speed for the selected sti...

Page 119: ... pH Buffers used in older calibrations will not have a solid background If calibrating with a standard buffer in MTC mode the pH value and temperature can be modified by pressing The values can be adjusted using the numeric keys Press to save the new values buffer solution one for rinsing the electrode and one for calibration If you are measuring in the acidic range use pH 7 01 or 6 86 as the firs...

Page 120: ...sage appears when the difference between the pH reading and the value of the selected calibration buffer is significant If the message is displayed check if you have selected the appropriate calibration buffer Wrong buffer temperature This message appears if the buffer temperature is out of the defined temperature range Clean the electrode or check the buffer Press to update calibration This messa...

Page 121: ...nformation Stores the current mV reading see section 7 4 2 Manual Logging or Starts the mV automatic log see section 7 4 1 Automatic Logging Enter the relative mV calibration screen see section 7 2 3 Relative mV Calibration Enter the mV setup screen Parameters are associated with mV measurement and calibration Allows the user to switch between the available measurement modes Titrator pH mV or ISE ...

Page 122: ...elative mV Offset Clear the relative mV offset and return to absolute mV measurement Press to clear the relative mV offset or to return to the previous screen 7 2 2 2 Logging Interval Set the logging interval sale ponpe com www ponpe com ...

Page 123: ...ability criteria Fast quicker results with less accuracy Medium medium speed results with medium accuracy Accurate slower results with high accuracy 7 2 2 4 Stirrer Configuration Set the stirrer configuration Stirrer 1 Stirrer 2 or Disabled sale ponpe com www ponpe com ...

Page 124: ... Speed The stirring speed for the selected stirrer can be set 7 2 3 mV Rel Calibration Press to accept the value Press to delete the last digit Press to cancel this operation and return to the previous screen sale ponpe com www ponpe com ...

Page 125: ...r more information Stores the current concentration reading see section 7 4 2 Manual Logging or Starts the ISE automatic log see section 7 4 1 Automatic Logging Enter the ISE calibration screen see section 7 3 3 ISE Calibration Enter the ISE setup screen Parameters are associated with ISE measurements and calibration Allows the user to switch between the available measurement modes Titrator pH mV ...

Page 126: ...libration Group Selecting the set of available standards to be used in calibration All standards the set of available standards includes the Standard Solutions and Custom Solutions Standards Group the set of available standards includes the standards selected by the user sale ponpe com www ponpe com ...

Page 127: ...al Point This option is available only if temperature compensation is enabled This option allows the user to set an isopotential point for the selected electrode Ion selective electrodes have different isopotential points The isopotential point is edited in ppm units only The isopotential point should be entered if it is known and if measurements are going to be made at several temperatures sale p...

Page 128: ...to invalidate the standard Press to edit the selected custom standard use the numeric keys to edit the standard 7 3 2 5 Edit Standard Group Select up to 5 standards from the available standards Predefined and Custom to be used during calibration Use the arrow keys to select the standard to be included removed in from the standard group sale ponpe com www ponpe com ...

Page 129: ...bration reminder will appear daily at specified time Periodic the calibration reminder will appear after the set time has elapsed since the lost calibration Disable the calibration reminder will not appear 7 3 2 7 Set Reminder Period If Daily or Periodic option was selected for the Calibration Reminder the reminder period must also be set For a daily reminder period the time of day can be set For ...

Page 130: ...n reminder and return to pH setup 7 3 2 8 Clear Calibration This option clears the existing ISE calibration If the calibration is cleared a new calibration must be done in order to take measurements Press to clear the previous calibration or to return to the previous screen 7 3 2 9 ISE GLP Data Displays the ISE calibration data sale ponpe com www ponpe com ...

Page 131: ...onstants press at any time to exit Ion Constants view For Custom ISE Press to edit the ion constants for the selected custom ISE Use the and keys to select the desired Ion constant and press to edit the value or to cancel operation Set the Ion Name up to 10 characters can be entered Set the appropriate molecular weight in g mol using the numeric keys Press to save the value or press to return to t...

Page 132: ...sired concentration unit for the measured ion or chemical compound The available concentration units are ppt g L ppm mg L ppb µg L mg mL M mol L mmol L w v or user defined 7 3 3 12 Logging Interval Set the logging interval to be used sale ponpe com www ponpe com ...

Page 133: ...riteria for the measured parameters Fast quicker results with less accuracy Medium medium speed results with medium accuracy Accurate slower results with high accuracy 7 3 3 14 ISE Significant Digits Select the number of significant digits to be displayed one x two xx or three xxx sale ponpe com www ponpe com ...

Page 134: ...ld also be recalibrated whenever the Calibrate Electrode message appears on the LCD Due to electrode conditioning time the electrode must be immersed for several seconds to stabilize The user will be guided step by step during calibration with easy to follow mes sages on the display This will make the calibration a simple and error free procedure PREPARATION Pour small quantities of the standard s...

Page 135: ...emperature compensation option is enabled the isopotential point of the electrode must be set in ISE Setup The current standard will be manually selected by the user from the available standards list The list of available standards depends of the Manual Entry setting To calibrate the instrument using Manual Entry Press from the main screen If the instrument was calibrated before and the calibratio...

Page 136: ... the pH mV ISE report and then press to activate deactivate it Each field marked by is an active field selected for the report Press to save the customized report 7 4 1 Automatic Logging The logging interval is set in the pH mV ISE setup screen Press to start the log The logging interval and name of logging file will be also displayed on the measure screen To stop the automatic logging press again...

Page 137: ... Manual Dispense 8 5 8 1 4 Purge Burette 8 5 8 2 Stirrer 8 6 8 3 Results 8 6 8 3 1 Review Last Titration Report 8 7 8 3 2 Review Available Reports 8 8 8 3 3 GLP Data 8 8 8 3 4 Instrumentation Data 8 9 8 3 5 Logging Interval pH mV ISE 8 10 8 3 6 Setup pH mV ISE Report 8 10 8 3 7 Setup Titration Report 8 10 sale ponpe com www ponpe com ...

Page 138: ...8 2 AUXILIARY FUNCTIONS sale ponpe com www ponpe com ...

Page 139: ...Burette screen press from the main titration screen Highlight the desired option and then press allows you to select the desired pump for burette operations it is only active if two pumps are connected 8 AUXILIARY FUNCTIONS sale ponpe com www ponpe com ...

Page 140: ...nected on the right side and the aspiration tube on the left side Note Before starting this operation the aspiration tube must be inserted in the titrant bottle A waste container should be placed under the dispensing tip to collect the waste solution To prime the burette select Prime Burette from the Burette screen Enter the number of rinses and press The number of burette rinses can be set betwee...

Page 141: ... Dispense screen will become active and the display will prompt you to enter the desired volume to be dispensed The manual dispense volume must be between the limits shown below 0 001 to 4 500 mL for a 5 mL burette 0 001 to 9 000 mL for a 10 mL burette 0 005 to 22 500 mL for a 25 mL burette 8 1 4 Purge Burette This option allows the burette to be emptied before cleaning and or storing the burette ...

Page 142: ...rned on and off by pressing The stirring speed is set within the method parameters see section 5 5 17 Stirring Speed During the titration process the stirring speed can be manually adjusted by using the and keys 8 3 Results From the Data Parameters screen you can access the following options sale ponpe com www ponpe com ...

Page 143: ...n Report screen The following option keys are available Review the titration graph The potentiometric titration curve is displayed If the Equivalence End Point option was selected the derivative curve 1st derivative 2nd derivative is simultaneously displayed Pressing will change the vertical axes scale units Print the titration report Return to the previous screen Keys can be used to scroll throug...

Page 144: ...report contains only the information selected in the Setup Titration Report and Setup pH mV ISE Report screens during report configuration The following option keys are available Review the selected graph Review the selected report Print the selected report Delete the selected report Return to the previous screen 8 3 3 GLP Data Enter up to 20 alphanumeric characters for each option from GLP Data s...

Page 145: ...3 4 Instrumentation Data Displays titrator configuration data Titrator Serial Number The serial number of the titrator base board Analog Board 1 and or 2 Serial Number The serial number of the analog board Pump 1 and or 2 Serial Number The serial number of the connected pump Titrator Software Version The current software version installed on the titrator Base Board Software Version The current sof...

Page 146: ...tion 7 3 Logging 8 3 6 Setup pH mV ISE Report Customize a unique report to record the pH mV and ISE measurements An asterisk means that it will be included in the report 8 3 7 Setup Titration Report Customize a unique report to record the titration results An asterisk means that it will be included in the titration report sale ponpe com www ponpe com ...

Page 147: ...sassembling the Burette 9 4 9 1 4 Assembling the Burette 9 4 9 1 5 Cleaning the Burette 9 5 9 1 6 Burette Preparation Filling with Titrant 9 7 9 2 Fuses Replacement 9 8 9 3 Peripherals 9 9 9 3 1 Connecting an External Display 9 9 9 3 2 Connecting an External PC Keyboard 9 9 9 3 3 Connecting a Printer 9 1 1 9 3 4 Connecting to a Computer 9 1 1 sale ponpe com www ponpe com ...

Page 148: ...9 2 MAINTENANCE PERIPHERALS sale ponpe com www ponpe com ...

Page 149: ...he burette is delivered with a 25 mL syringe inside and with all of the accessories mounted see section 2 1 Unpacking for burette assembly details The burette assembly consists of a rigid housing which holds the glass syringe a 3 2 way value and titrant tubing 9 1 2 Changing the Burette Remove the burette from the pump assembly by sliding it forward and then slide the new burette into place see th...

Page 150: ...k 4 from the burette holder Unscrew the fitting 2 Remove the tube 9 1 4 Assembling the Burette To attach the dispensing tube and the aspiration tube follow these steps Insert the flat shaped end of the dispensing tube into the valve outlet and screw in the fitting so that the highest of its 9 cuts stays vertically in the final position 2 Bend the tube up into the vertical position to enter the hig...

Page 151: ...onized water or solvent and allow the air to replace the liquid in the burette This will clean the aspiration tube If this simple cleaning procedure is not adequate continue with these steps Slide the burette out from the pump assembly Remove the dispensing and aspiration tubes Clean them separately or insert new ones Remove the protective cap from the bottom of the burette assembly by using the s...

Page 152: ...e burette with bare hands or greasy materials Reinsert the piston into the syringe Reinsert the syringe by screwing it in the valve with your fingers Reinsert the protective cap to the bottom of the burette assembly Carefully position the cap into the burette Slide the burette into the burette stand Notice the position of the piston shaft to the pump couple Priming the burette three times with new...

Page 153: ...Press Insert the aspiration tube into the titrant bottle only when the piston is going down and has reached about from the upper end To avoid the presence of the air bubbles inside the burette make sure to have a continuous liquid flow inside the burette A little air just above the liquid level at the first filling is normal The next filling will evacuate all of the air no air will be left in the ...

Page 154: ... fuses for recommended fuses replacement please see the label located above the power switch Close the fuse holder lid Connect the power cord Note For other maintenance operations please contact your dealer or the nearest Hanna Customer Service Center 9 3 Peripherals Warning Connection disconnection of POWER CORD PUMP ASSEMBLY EXTERNAL PC DISPLAY PRINTER RS232 INTERFACE EXPANSION DEVICE must only ...

Page 155: ...cted with a 15 pin cable as presented below Connect the external display to the display socket Turn on the titrator and then the external display 9 3 2 Connecting an External PC Keyboard This connection allows you to use an external PS 2 PC Keyboard in addition to the titrator s keypad Connect an external PC Keyboard PS 2 connector sale ponpe com www ponpe com ...

Page 156: ... F 4 Function Key F 5 Option Key 1 from left to right Function Key F 6 Option Key 2 from left to right Function Key F 7 Option Key 3 from left to right Function Key F 8 Option Key 4 from left to right Function Key F 9 Option Key 5 from left to right Function Key F 10 Arrow Key Up Arrow Key Down Arrow Key Left Arrow Key Right Page Up Page Down Numeric Keys 0 to 9 to Tab Enter Alphanumeric Keys Allo...

Page 157: ... Warning The titrator and the external printer must be both turned OFF before they are connected Connect the external printer to the standard 25 pin Socket Turn on the titrator and then the printer 9 3 4 Connecting to a Computer The titrator can be connected to a computer using a USB cable HI 900 PC application needs to be installed on the PC sale ponpe com www ponpe com ...

Page 158: ...port on the PC Select the USB Communication screen on the titrator following the path General Options USB Link with PC Launch the HI 900 PC application and then select the appropriate USB Port on the PC The HI 900 PC application allows the transfer of methods and reports between the titrator and PC sale ponpe com www ponpe com ...

Page 159: ...A1 1 APPENDIX 1 Appendix 1 Contents A1 TECHNICAL SPECIFICATIONS A1 3 sale ponpe com www ponpe com ...

Page 160: ...A1 2 APPENDIX 1 sale ponpe com www ponpe com ...

Page 161: ...guages English Portuguese Spanish Titration Methods up to 100 standard and user methods Burette size auto detection and interchangeable burettes The titrator automatically detects the size of the burette when it is slid in the pump assembly Propeller Stirrer with Programmable Stir Speed The stirring speed can be set between 100 and 2500 RPM with 100 RPM resolution Flow Rate user selectable see Sec...

Page 162: ...up to 100 complete titration report and pH mV ISE reports Files Copied to and Restored from USB Storage Device Standard Methods User Methods Titration and pH mV ISE Logging Reports and Bitmap Files can be transferred to a PC using a USB storage device Peripheral Units External VGA Display External PC Keyboard Printer PC via USB Interface GLP Conformity Good Laboratory Practice and Instrumentation ...

Page 163: ...A2 1 Applicability Domain A2 3 A2 2 Method Principles A2 3 A2 3 Example of a Back Titration A2 3 A2 3 1 Introduction A 2 3 A2 3 2 Setting Up the Method Parameters A 2 4 A2 3 3 Preparing the Sample A 2 5 A2 3 4 Perform the Titration A 2 5 sale ponpe com www ponpe com ...

Page 164: ...A2 2 APPENDIX 2 sale ponpe com www ponpe com ...

Page 165: ... calculated using this value A2 3 Example of a Back Titration An example of a back titration is determining the neutralizing capacity of antacid A2 3 1 Introduction An excess of stomach acid primarily HCl causes heartburn and acid indigestion Commercial antacids active ingredient is a basic salt such as Mg OH 2 milk of magnesia NaHCO3 sodium bicarbonate CaCO3 calcium carbonate or Al OH 3 aluminum ...

Page 166: ...0 000 mL Pre Titration Stir Time 5 Sec Measurement Mode Signal Stability delta E 0 3 mV delta t 1 5 Sec t min wait 5 Sec t max wait 15 Sec Electrode Type pH Calculations Sample Calc by Weight Titrant 1 Units M mol L Titrant 2 Units M mol L Final Result Units g g Titrant 1 Name HCl Titrant 1 Conc 1 M mol L Titrant 2 Name NaOH Titrant 2 Conc 1 M mol L Analyte Size 0 5 g Analyte Entry Manual Titrant ...

Page 167: ...sible to the bottom of the beaker If necessary add more distilled or deionized water so that the pH electrode bulb is completely immersed in the sample and the reference junction of the electrode is 5 6 mm below the surface A2 3 4 Perform the Titration When the method is selected the main screen displays Antacid Power press The titrator will prompt for the sample weight Enter the exact weight valu...

Page 168: ...has ceased then boil it for 1 2 minutes Some of the inactive tablet material may not dissolve however this should not interfere with the titration Cool the solution to room temperature and put the beaker under the stirrer assem bly Lower the stirrer assembly until it rest on its positioning collar Press to proceed to the second phase of the analysis The results will be displayed on the screen sale...

Page 169: ...3 Multiple Equivalence Point Titration A3 MULTIPLE EQUIVALENCE POINTS A3 3 A3 1 Applicability Domain A3 3 A3 2 Performing a Titration A3 3 A3 3 Example of a Multiple Equivalence Point Titration A3 4 sale ponpe com www ponpe com ...

Page 170: ...A3 2 APPENDIX 3 sale ponpe com www ponpe com ...

Page 171: ...wo equivalence points in aqueous medium A3 2 Performing a Titration Set up the method parameters as follows Set the end point mode to equivalence end point mV or pH Set the number of equivalence points up to 5 points can be detected Select the end point determination first or second derivative The rest of the method parameters can be modified if needed and save the method Note In the method calcul...

Page 172: ...ith Sodium Hydroxide During this type of titration the user is able to view the following information After first equivalence point is detected the titration screen will show and the number of equivalence points detected By pressing the titrator will display EQ Points Report This screen contains information about the detected equivalence points sale ponpe com www ponpe com ...

Page 173: ... titrant dispensed The volumes of each additional point marked with an x are calculated as the difference between the total volume dispensed to reach the current equivalence point and the sum of the previously detected equivalence points The concentration is calculated with the formula selected in the Calculations option from the View Modify Method screen sale ponpe com www ponpe com ...

Page 174: ...A3 6 APPENDIX 3 sale ponpe com www ponpe com ...

Page 175: ... 1 APPENDIX 4 Appendix 4 Linked Method A4 LINKED METHOD A4 3 A4 1 Creating a Linked Method A4 3 A4 2 Selecting a Linked Method A4 6 A4 3 Running a Linked Titration Method A4 7 sale ponpe com www ponpe com ...

Page 176: ...A4 2 APPENDIX 4 sale ponpe com www ponpe com ...

Page 177: ... a linked method use the following procedure From the main screen press and use the arrow keys to highlight the first method Press Press to access the Method Options screen Use the arrow keys to highlight Linked To The Linked To option allows you to select the second titration method If No Link is selected only the current method will run sale ponpe com www ponpe com ...

Page 178: ... The second titration can be started either automatically or manually If Automatically is selected the second titration will start immediately after the first titration has completed No user input is required If Manually is selected user input is required to start the second method sale ponpe com www ponpe com ...

Page 179: ...n If both methods are using the same type of calculation sample calculation by volume or by weight the option for Same as Previous is available for Method 2 This allows the same weight or volume to be used in both calculations Same as Previous is not available if different types of calculations are being used sale ponpe com www ponpe com ...

Page 180: ...urn to the main screen A4 2 Selecting a linked method All linked methods are moved to the top of the user method list and are noted with next to the method number When a method is linked only the first method can be selected and the second method is indented below it sale ponpe com www ponpe com ...

Page 181: ...d Titration Method Press to begin the linked titration After the completion of the first titration the selected pump will return to the home position before the second titration is started The titrator will either start the second titration auto matically or wait for user input sale ponpe com www ponpe com ...

Page 182: ...4 8 APPENDIX 4 When the second titration has finished the results for both titrations will be shown on the screen To start a new titration press to return to the main screen sale ponpe com www ponpe com ...

Page 183: ... 7 Electrode Storage Solutions A 5 4 A5 1 8 Electrode Storage Solutions in FDA Approved Bottle A 5 4 A5 1 9 Refilling Electrolyte Solutions A 5 4 A5 1 10 Refilling Electrolyte Solutions in FDA Approved Bottle A 5 5 A5 1 11 ORP Pretreatment Solutions A 5 5 A5 1 12 Titration Reagents A 5 5 A5 1 13 Ion Selective Electrode Calibration Solutions A 5 5 A5 2 Sensors A5 6 A5 2 1 pH Electrodes A 5 6 A5 2 2...

Page 184: ...A5 2 APPENDIX 5 sale ponpe com www ponpe com ...

Page 185: ...4L pH 4 01 Buffer Solution 500 mL HI 8006L pH 6 86 Buffer Solution 500 mL HI 8007L pH 7 01 Buffer Solution 500 mL HI 8009L pH 9 18 Buffer Solution 500 mL HI 8010L pH 10 01 Buffer Solution 500 mL A5 1 3 pH Technical Calibration Solutions HI 5016 pH 1 68 Buffer Solution 500 mL HI 5003 pH 3 00 Buffer Solution 500 mL HI 5004 pH 4 01 Buffer Solution 500 mL HI 5068 pH 6 86 Buffer Solution 500 mL HI 5007...

Page 186: ...olution 230 mL HI 7074L Inorganic Cleaning Solution 500 mL HI 7077M Oil Fat Cleaning Solution 230 mL HI 7077L Oil Fat Cleaning Solution 500 mL A5 1 6 Electrode Cleaning Solutions in FDA Approved Bottle HI 8061M General Purpose Solution 230 mL HI 8061L General Purpose Solution 500 mL HI 8073M Protein Cleaning Solution 230 mL HI 8073L Protein Cleaning Solution 500 mL HI 8077M Oil Fat Cleaning Soluti...

Page 187: ...agent 1 L HI 70440 0 02 N Stabilized Iodine Titration Reagent 1 L HI 70441 0 04 N Stabilized Iodine Titration Reagent 1 L HI 70448 0 02 M AgNO3 Titration Reagent 1 L HI 70449 0 02 M EDTA Titration Reagent 1 L HI 70455 0 01 N NaOH Titration Reagent 1 L HI 70456 0 1 N NaOH Titration Reagent 1 L HI 70457 1 N NaOH Titration Reagent 1 L HI 70458 0 01 M H2SO4 Titration Reagent 1 L HI 70459 0 05 M H2SO4 ...

Page 188: ... 1 pH Electrodes HI 1043B Glass body double junction refillable combination pH electrode Use strong acid alkali HI 1053B Glass body triple ceramic conic shape refillable combination pH electrode Use emulsions HI 1083B Glass body micro Viscolene nonrefillable combination pH electrode Use biotechnology micro titration HI 1131B Glass body single junction refillable combination pH electrode Use genera...

Page 189: ...ombination pH electrode Use milk yogurt and cream FC 220B Glass body single junction refillable combination pH electrode Use creams fruit juices and sauces FC 911B Plastic body PVDF double junction refillable combination pH electrode Use creams fruit juices and sauces HI 1413B Glass body single junction flat tip Viscolene combination pH electrode Use surfaces skin leather paper emulsions A5 2 2 OR...

Page 190: ... reference half cell electrode refillable with 4mm plug with 1m 3 3 cable Use general purpose with constant temperature range A5 2 4 Ion Selective Electrodes HI 4101 Ammonia ISE HI 4002 HI 4102 Bromide ISE HI 4003 HI 4103 Cadmium ISE HI 4004 HI 4104 Chloride ISE HI 4105 Carbon Dioxide ISE HI 4007 HI 4107 Chloride ISE HI 4008 HI 4108 Cupric ISE HI 4009 HI 4109 Cyanide ISE HI 4010 HI 4110 Fluoride I...

Page 191: ...tube guide Tube locks Tool for burette cap re moval Light spectrum protection screen Overhead Stirrer Propeller Stirrer support with positioning collar and positioning screw Stirrer stand Burette blank support Pump Assembly and Burette Blank support locking screw with plastic head Temperature Probe Power Cable USB Cable A5 3 Titrator components sale ponpe com www ponpe com ...

Page 192: ...A5 10 APPENDIX 5 USB Storage Device Shorting cap Instruction Manual Binder H I 90 1 90 2 HI 900 Series Titration Systems Ww w h ann ainst c om sale ponpe com www ponpe com ...

Page 193: ...A5 11 APPENDIX 5 ...

Page 194: ...A5 12 APPENDIX 5 MAN902C 10 10 ...

Page 195: ...1 General Titration Applications Brochure HI 902 Color AUTOMATIC POTENTIOMETRIC TITRATOR Revision 2 3 sale ponpe com www ponpe com ...

Page 196: ...1 2 INTRODUCTION ...

Page 197: ...abilized with an accuracy of 0 0001 grams Remove the beaker from the balance and add distilled water to the 50 mL mark on the beaker Place the beaker under the stirrer assembly and immerse the pH electrode temperature probe and stirrer Ensure that the reference junction of the pH probe is 5 6 mm below the surface If necessary add extra distilled water Press Start You will be prompted to enter the ...

Page 198: ...Flow Rate 25 mL 50 mL min Signal Averaging 1 Reading Significant Figures XXXXX Calculations Calculations Stdz Titrant by Weight Titrant units N eq L Titrant volume dosed V L Standard weight 0 200 g titrant standard 1 000 eq mol MW of standard 204 23 g mol Results Titration Report Method Name 0 1N NaOH Titr Conc Time Date 11 38 April 21 2010 Titration ID Ti_00010 Titration Results Method Name 0 1N ...

Page 199: ... electrode temperature probe and stirrer Ensure that the reference junction of the pH probe is 5 6 mm below the surface If necessary add extra distilled water Press Start The titrator will start the analysis At the end of the titration after detection of the equivalence point titration completed will appear with the titrant concentration The result is expressed in N eq L of hydrochloric acid Remov...

Page 200: ...d conc 0 100 eq L Results Titration Report Method Name 0 1N HCl Titr Conc Time Date 14 28 April 21 2010 Titration ID Ti_00011 Titration Results Method Name 0 1N HCl Titr Conc Time Date 14 28 April 21 2010 Analyte size 10 000 mL End Point Volume 9 979 mL pH Equivalence Point 5 059 Results 0 10215 N eq L Initial and Final pH 12 135 to 4 989 Titration Duration 2 45 mm ss Titration went to Completion ...

Page 201: ...HI 70425 and 1 5 g of potassium iodide HI 70468 Place the beaker under the stirrer assembly and immerse the ORP electrode and stirrer Ensure that the reference junction of the ORP electrode is 5 6 mm below the surface If necessary add extra distilled water Press Start You will be prompted to enter the analyte size weight of KIO3 Use the numeric keypad to enter the exact weight and press Enter to s...

Page 202: ...its M mol L Titrant volume dosed V L Standard weight 0 350 g Dilution factor 0 10 Final dilution volume 100 000 mL Aliquot volume 10 000 mL titrant standard 6 000 mol mol MW of standard 214 00 g mol Results Titration Report Method Name 0 1M Na2S2O3 Titr Conc Time Date 08 52 April 22 2010 Titration ID Ti_00003 Titration Results Method Name 0 1M Na2S2O3 Titr Conc Time Date 08 52 April 22 2010 Analyt...

Page 203: ...to a 100 mL volumetric flask Add approximately 80 mL of distilled water and mix Dissolve completely before bringing to volume Use a class A volumetric pipette to transfer exactly 10 00 mL of prepared standard solution to a clean 100 mL plastic beaker and 25 mL of 25 sulfuric acid solution HI 70444 Use distilled water to bring the total volume to about 50 mL Place the beaker under the stirrer assem...

Page 204: ...ng Speed 1400 rpm Potential Range 2000 0 to 2000 0 mV Volume Flow Rate 25 mL 50 mL min Signal Averaging 1 Reading Significant Figures XXXXX Calculations Calculations Stdz Titrant by Weight Titrant units M mol L Titrant volume dosed V L Standard weight 0 490 g Dilution factor 0 10 Final dilution volume 100 000 mL Aliquot volume 10 000 mL titrant standard 6 000 mol mol MW of standard 294 18 g mol Re...

Page 205: ...mL glass beaker and add distilled water to the 100 mL mark on the beaker To the beaker add 10 mL of 1 5M nitric acid HI 70427 Place the beaker under the stirrer assembly and immerse the electrodes and stirrer Ensure that the reference junction of the ORP electrode is 5 6 mm below the surface If necessary add extra distilled water Press Start You will be prompted to enter the analyte size weight of...

Page 206: ...lations Stdz Titrant by Weight Titrant units M mol L Titrant volume dosed V L Standard weight 0 200 g Dilution factor 0 05 Final dilution volume 100 000 mL Aliquot volume 5 000 mL titrant standard 1 000 mol mol MW of standard 58 440 g mol Results Titration Report Method Name 0 02M AgNO3 Titr Conc Time Date 08 52 June 30 2010 Titration ID Ti_00003 Titration Results Method Name 0 02M AgNO3 Titr Conc...

Page 207: ...1N Hydrochloric Acid Titrant Concentration Use a class A volumetric pipette to transfer exactly 50 00 mL of sample to a clean 100 mL plastic beaker Place the beaker under the stirrer assembly and immerse the pH electrode temperature probe and stirrer Ensure that the reference junction of the pH probe is 5 6 mm below the surface Press Start The titrator will begin the analysis At the end of titrati...

Page 208: ...Date 09 04 April 18 2010 Titration ID Ti_00004 Titration Results Method Name Alkalinity of Water Time Date 09 04 April 18 2010 Analyte size 50 000 mL End Point Volume 9 336 mL pH Fixed End Point 4 500 Results 934 44 mg L Initial and Final pH 10 232 to 4 419 Titration Duration 3 23 mm ss Titration went to Completion Operator name ____________________________ sale ponpe com www ponpe com ...

Page 209: ...1N Sodium Hydroxide Titrant Concentration Use a class A volumetric pipette to transfer exactly 50 00 mL of sample to a clean 100 mL plastic beaker Place the beaker under the stirrer assembly and immerse the pH electrode temperature probe and stirrer Ensure that the reference junction of the pH probe is 5 6 mm below the surface Press Start The titrator will begin the analysis At the end of titratio...

Page 210: ...ate 09 15 April 22 2010 Titration ID Ti_00005 Titration Results Method Name Acidity of Water Time Date 09 15 April 22 2010 Analyte size 50 000 mL End Point Volume 5 879 mL pH Fixed End Point 8 300 Results 588 43 mg L Initial and Final pH 2 465 to 8 398 Titration Duration 3 42 mm ss Titration went to Completion Operator name ____________________________ sale ponpe com www ponpe com ...

Page 211: ...ace the beaker under the stirrer assembly and immerse the silver sulfide ISE reference electrode temperature probe and stirrer Ensure the electrodes are 5 6 mm below the surface Press Start The titrator will begin the analysis At the end of the titration after detection of the equivalence point titration completed will appear with the chloride concentration The result is expressed in mg L as chlor...

Page 212: ... April 23 2010 Titration ID Ti_00029 Titration Results Method Name Chloride in Water Time Date 09 20 April 23 2010 Analyte size 100 00 mL End Point Volume 4 781 mL mV Equivalence Point 280 3 Results 33 897 mg L Initial and Final mV 194 8 to 298 5 Titration Duration 1 24 mm ss Titration went to Completion Operator name ____________________________ sale ponpe com www ponpe com ...

Page 213: ...Place the beaker under the stirrer assembly and immerse the pH electrode temperature probe and stirrer Ensure that the reference junction of the pH probe is 5 6 mm below the surface If necessary add extra distilled water Press Start The titrator will start the analysis At the end of titration after detection of the equivalence point titration completed will appear together with the base concentrat...

Page 214: ...e 13 04 April 23 2010 Titration ID Ti_00008 Titration Results Method Name Neutralization w H2SO4 Time Date 13 04 April 23 2010 Analyte size 10 000 mL End Point Volume 9 562 mL pH Equivalence Point 7 966 Results 95 620 meq L Initial and Final pH 11 655 to 6 248 Titration Duration 3 26 mm ss Titration went to Completion Operator name ____________________________ sale ponpe com www ponpe com ...

Page 215: ...about 50 mL Place the beaker under the stirrer assembly and immerse the pH electrode temperature probe and stirrer Ensure that the reference junction of the pH probe is 5 6 mm below the surface If necessary add extra distilled water Press Start The titrator will start the analysis At the end of the titration after detection of the equivalence point titration completed will appear with the acid con...

Page 216: ...te 13 04 April 23 2010 Titration ID Ti_00009 Titration Results Method Name Neutralization w NaOH Time Date 13 04 April 23 2010 Analyte size 10 000 mL End Point Volume 15 970 mL pH Equivalence Point 8 431 Results 159 70 meq L Initial and Final pH 2 675 to 10 316 Titration Duration 3 20 mm ss Titration went to Completion Operator name ____________________________ sale ponpe com www ponpe com ...

Page 217: ...ead from the balance after each dose The following information is needed to verify the accuracy of the dosing system The temperature of the dispensed water The atmospheric air pressure The density of the weight used to calibrate the balance Note This procedure can be repeated on pump 2 Method Parameters Name Troubleshooting 1 Method Revision 2 3 Titration Type Standard Titration Analog Board Analo...

Page 218: ...t on Analog Board 1 The titrator should display ATC 70 0 0 4 C with no fluctuation or drift Note This procedure can be repeated on analog 2 Temperature mV Channel Logging Procedure Connect the shorting cap to the BNC socket on Analog Board 1 Connect the HI 762000C 0 C temperature key to the RCA socket temperature sensor input on Analog Board 1 Once on the main screen select Mode ensure that Analog...

Page 219: ...ad from the balance after each dose The following information is needed to verify the accuracy of the dosing system The temperature of the dispensed water The atmospheric air pressure The density of the weight used to calibrate the balance Note This procedure can be repeated on pump 2 Method Parameters Name Troubleshooting 2 Method Revision 2 3 Titration Type Standard Titration Analog Board Analog...

Page 220: ...kage and burette and tubing for air bubbles Repeat the measurements The table below contains the settings to be used for other burette volumes Burette Volume Dosing Type Pre Titr Volume Max Titr Volume 5 mL 10 mL 25 mL 4 000 mL 8 000 mL 20 000 mL 4 000 mL 8 000 mL 20 000 mL 8 000 mL 16 000 mL 40 000 mL Stirring Device Fast Check Procedure From the titrators main screen press stir on the keyboard a...

Page 221: ...mpletely For sparkling samples remove the CO2 by passing nitrogen through it using an ultrasonic bath or by stirring and applying vacuum Use a class A volumetric pipette to transfer exactly 100 00 mL of sample to a clean 150 mL glass beaker Place the beaker under the stirrer assembly and immerse the pH electrode temperature probe and stirrer Ensure that the reference junction of the pH probe is 5 ...

Page 222: ...e volume 100 000 mL Results Titration Report Method Name Concentration of H3PO4 Time Date 10 11 April 23 2010 Titration ID Ti_00014 Titration Results Method Name Concentration of H3PO4 Time Date 10 11 April 23 2010 Analyte size 100 000 mL Equivalence point 1 pH 4 677 Volume 4 397 mL Results 4 3972e 3 mol L Equivalence point 2 pH 8 916 Volume 4 429 mL Results 4 4293e 3 mol L Titration Duration 6 01...

Page 223: ...1 TITRATION THEORY TITRATION THEORY HI 901 and HI 902 AUTOMATIC POTENTIOMETRIC TITRATOR sale ponpe com www ponpe com ...

Page 224: ...2 TITRATION THEORY sale ponpe com www ponpe com ...

Page 225: ...2 2 1 Acid Base Titrations 9 2 2 2 Argentometric Titrations 10 2 2 3 Complexometric Titrations 10 2 2 4 Ion Selective Titrations 11 2 2 5 Non aqueous Solvent Acid Base Titrations 11 2 2 6 Precipitation Titrations 12 2 2 7 Redox Titrations 12 2 2 8 Karl Fischer Titration 13 2 3 Titrations According to The Titration Sequence 13 2 3 1 Back Titrations 13 2 3 2 Multiple Endpoint Titrations 14 3 INTRODU...

Page 226: ... Preparation Errors 17 4 3 2 2 Dispensing Errors 18 4 3 3 Chemical Reaction Errors 18 4 3 4 Endpoint Determination Errors 18 5 CALCULATIONS 19 5 1 Sample Calculation 19 5 2 Standardize Titrant 19 5 3 Blank Titration 20 5 4 Multiple Endpoint Titration 20 5 5 Back Titration 21 6 GLOSSARY 22 sale ponpe com www ponpe com ...

Page 227: ...r by some other physical measurement Titrations cannot be used to determine the quantity of all analytes The chemical reaction between the titrant and analyte must fulfill four requirements The reaction must be fast and occur within approximately one second after the titrant is added The reaction must go to completion The reaction must have well known stoichiometry reaction ratios A convenient end...

Page 228: ...training Suitability to measure major components of a mixture or product Automation can reduce time and labor spent on each analysis Some disadvantages of titrations are Time it takes to prepare standards and titrants Good technique is required to achieve precise results training and practice required Not suitable for determining trace or minor components of a mixture or product Limited dynamic ra...

Page 229: ... amperometrically titrated using a precipitation complexation or redox reaction Some metal ions and species that can be determined in this manner include silver barium halides potassium magnesium palladium molybdate sulfate tungstate zinc bismuth cadmium fluoride indium thallium iodine and gold Figure 1 shows four amperometric titrations and their endpoints In graph A the analyte is electroactive ...

Page 230: ... Highly colored indicators that change color during the course of the titration are available for many titrations More accurate data on the titration curve can be obtained if the light absorption is monitored instrumentally using a light source a simple monochromator and a photodetector rather than visually determining the color or light absorption change Light absorption by either an indicator or...

Page 231: ...ains a list of some aqueous acid base chemical indicators as well as the pH range the pKa and the expected color acid and base form When choosing the proper indicator you should select one that has a pKa as close to the endpoint of the titration When chemical indicators are not suitable a potentiometric pH titration can also be used The pH of the solution is plotted versus the volume of titrant ad...

Page 232: ...tion can be easily followed with a silver ISE or chloride ISE for chloride titrations and a reference electrode Figure 5 shows the titration of 50 mL of 0 1N NaCl with 0 1N AgNO3 The potentiometric signal is from a chloride ISE and is plotted as pCl log Cl 2 2 3 Complexometric Titrations A complex is a species where a central metal ion is covalently bonded to one or more electron donating groups c...

Page 233: ...ting fluoride with an aluminum titrant using a fluoride ISE chloride with silver nitrate using a chloride ISE sodium with a sodium ISE etc The equivalence point can be determined by plotting the mV value vs the amount of titrant added 2 2 5 Non aqueous Solvent Acid Base Titrations Non aqueous solvents must be used to titrate very weak acids and bases due to the inherent leveling effect water has o...

Page 234: ... unstable potentials 2 2 6 Precipitation Titrations Precipitation titrations allow for faster analysis compared to the old gravimetric analysis where a precipitate is formed filtered dried and weighed to analyze a compound Typically silver halides silver thiocyanate and a few mercury lead and zinc salts are titrated using this method The chemical reactions must form an insoluble salt and precipita...

Page 235: ... products organic and inorganic compounds chemicals solvents and gases petroleum and plastic products as well as paints and adhesives The KF method is verifiable and can be fully documented As a result Karl Fischer titration is the standard method for analysis of water in a multitude of samples as specified by numerous organizations including the Association of Official Analytical Chemists the Uni...

Page 236: ...has a different reduction potential complexometric where different species are separately titratable and acid base using polyprotic acids the pKa of the different protons varies enough to separate them Figure 9 shows three different types of multiple endpoint titrations A shows the titration of a polyprotic acid The different acid strengths of the first and second proton can be determined B illust...

Page 237: ...own concentration A visual or instrumental indicator for detecting the completion of the reaction A typical manual titration consists of the following steps 1 A volumetric pipette is typically used to add a known volume of sample to the flask 2 An indicator solution or instrument probe is added to the flask 3 A burette is used to measure the addition of titrant to the flask and dispense titrant in...

Page 238: ...h in the burette pump minimal piston seal flexing precision ground inner diameter of the glass syringe a low dead volume valve minimal evaporation permeation and chemically resistant tubing Apparatus required for automatic titration include An automatic titrator equipped with a burette A beaker An electronic stirring system either a propeller stirrer or a magnetic stir bar and stir plate Volumetri...

Page 239: ...sentative sample Sample changed or was contaminated during collection storage or transfers Poor technique when transferring sample to beaker or flask Errors in the balance calibrate and check balance regularly 4 3 2 Errors with Titrant and Standard 4 3 2 1 Preparation Errors Incorrect preparation due to Poor technique in weighing the salt or when transferring to volumetric glassware Low purity of ...

Page 240: ...ive The inflection point of the titration curve mV vs Volume is normally assumed to be the equivalence point The first derivative is often used to determine the inflection point The maximum value of the first derivative dmV vs dV corresponds to the theoretical equivalence point During a titration it is rare to have a data point exactly at the first derivative maximum the maximum value is determine...

Page 241: ...ample Concentration g 100mL V titrant Volume of titrant L C titrant Titrant Concentration eq L Ratio Equivalence ratio of analyte titrant mol analyte eq titrant FW analyte Formula Weight of the Analyte g mol V sample Volume of Sample mL 5 2 Standardize Titrant Titrant standardization is the second most important calculation in titrations A primary standard is titrated in order to determine the con...

Page 242: ... titrant used in the blank titration should be subtracted from the regular titration titrant volume C Sample Sample Concentration g 100g C titrant Titrant Concentration eq L V sample Volume of Titrant required for the sample L V blank Volume of Titrant required for the blank L Ratio Equivalence ratio of analyte titrant mol analyte eq titrant FW analyte Formula Weight of the Analyte g mol m sample ...

Page 243: ... mL 5 5 Back Titration The equation used in back titration calculations is also similar to the equation for a blank titration Instead of subtracting the initial amount of titrant needed to react with the blank the amount of second titrant needed to react with the excess titrant added in the first titration is subtracted from the amount of the first titrant added The difference between the two amou...

Page 244: ...ration A type of titration where an excess amount of titrant is added to a sample forcing a sluggish reaction to go to completion The excess reagent is then back titrated with a second titrant Base A chemical species that can accept one or more protons hydrogen ions Biamperometric Indication Uses a double platinum pin electrode to measure the current flow through a titration solution Bivoltametric...

Page 245: ...al titrations chemical indicators have been replaced with electrometric indicators which are used with automatic titrators Inflection Point The point on a titration curve were the second derivative curve changes signs Ion Selective Electrode ISE An electrode that responds to a specific ion The electrode potential is proportional to the concentration or activity of that ion in the solution being me...

Page 246: ...yprotic Acid Acids that are capable of donating more than one proton per acid molecule Potentiometric Titration A titration in which the endpoint is determined by monitoring the voltage of the solution using an electrode Precipitation Titration A titration in which the analyte reacts with the titrant to form an insoluble compound The endpoint is typically detected with an ISE sensitive to either t...

Page 247: ...eaction to occur Titration A quantitative volumetric procedure used in analytical chemistry to determine the concentration of an analyte in solution The concentration of the analyte is determined by slowly adding a titrant to the solution As the titrant is added a chemical reaction between the titrant and the analyte occurs Titration Curve A graph containing the physical data obtained for a titrat...

Page 248: ...26 TITRATION THEORY Titr THEORY 901 902 04 10 ...

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