Hanna Instruments HI 903 Quick Start Manual Download

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TITRATION THEORY

Summary of Contents for HI 903

Page 1: ...1 QUICK START GUIDE HI 903 KARL FISCHER VOLUMETRIC TITRATOR Revision 1 0 ...

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

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

Page 4: ...4 QUICK START GUIDE ...

Page 5: ... between the pins of the electrode The endpoint detection algorithm incorporated in the HI 903 analyzes both the electrode response to individual additions of titrant and the shape of the entire titration curve in order to determine the endpoint of the titration Titration reports and methods can be transferred to a PC via a USB interface saved to a USB flash drive or printed directly from the titr...

Page 6: ...s check that the titrant solvent and waste bottles as well as the titration beaker are properly assembled 5 Always wipe up spills and splashes immediately 6 Avoid the following environmental working conditions Severe vibrations Direct sunlight Atmospheric relative humidity above 80 non condensing Environment temperatures below 10 C and above 40 C Near heating or cooling sources Explosion hazards 7...

Page 7: ...7 QUICK START GUIDE TITRATOR CONNECTIONS Front View Rear View ...

Page 8: ...backlit color display The Standby Mode screen is shown below with short explanations The user interface contains several screens In each screen many information fields are present at the same time The information is displayed in an easy to read manner using different size fonts Virtual option keys describe the function performed when the corresponding soft key is pressed ...

Page 9: ...xtual help can be accesed at any time and it provides useful information about the current screen METHODS The HI 903 Karl Fischer titrator can store up to 100 methods these include up to 90 stan dard methods Standard Methods Each titrator is supplied with a customized package of standard methods Standard method packs are developed at Hanna Instruments laboratories to meet analysis requirements of ...

Page 10: ...he tube and insert it in the waste bottle or separate waste container From the Idle screen press Highlight the Prime Burette option and then press Enter the number of burette rinses At least 3 rinses with the solution used for titration are recommended allowing air bubbles to be evacuated Press to start The message Executing will be displayed Note Make sure you have continuous liquid flow inside t...

Page 11: ...arameters from the standard methods can be changed For this titration only the KF titrant concentration value and the size of the solvent sample need to be entered as in the screen shown below To accomplish this Highlight Titrant option from the View Modify Method screen and then press The Karl Fischer Titrants screen will be displayed Press Highlight Standardized Titrant Concentration and press I...

Page 12: ...will enter Pre Titration mode start the magnetic stirrer and begin dosing titrant into the titration beaker If no titrant can be seen moving through the anti diffusion tip after several doses press and verify that no titrant is leaking from the burette housing or from the dispensing tube fittings Once all residual moisture has been reacted endpoint potential is reached the titra tor will enter Dri...

Page 13: ...uld be added using a class A pipette Note When adding samples using the weighing boat pipette or syringe without needle the septum has to be removed Therefore the adding operation should be performed quickly in order to avoid the prolonged exposure of the beaker to atmospheric moisture Performing a Titration From the main screen press for analyzing a sample or for titrant stan dardization You will...

Page 14: ...the end point potential for the selected stability time When the titration has ended the titrator will display the final concentration of the moisture together with the basic titration information To view the custom report or titration graph press To view statistics of multiple analyses press For titrant standardizations press to update the active titrant with the displayed standardization result ...

Page 15: ...ng the information transfer to the printer the message Printing will be displayed on the screen Press to return to the Data Parameters screen Press again to return to the main screen Saving the data on a USB storage device This feature allows saving the results of titrations or drift logging sessions on a USB storage device Insert the USB storage device into the USB socket From the Idle screen pre...

Page 16: ...tor Name KF Technician Electrode Name Probe 1 Field 1 Any text Field 2 Any text Field 3 Any text Titrator Software Version v1 0 Base Board Software Version v2 6 Pump Software Version v1 4 Titrator Serial Number 12345678 Analog Board Serial Number 12345678 Pump Serial Number 12345678 Analog Calibration Date Aug 22 2010 Method Parameters Name Moisture in Oil Method Revision 1 0 Type Sample Analysis ...

Page 17: ...78 403 0 00 00 08 6 0 0228 402 5 00 00 09 7 0 0278 402 4 00 00 11 8 0 0328 402 7 00 00 12 9 0 0378 402 5 00 00 14 10 0 0428 402 9 00 00 16 256 0 9904 169 7 00 06 45 257 0 9904 177 4 00 06 47 258 0 9904 173 7 00 06 48 259 0 9904 171 1 00 06 50 260 0 9904 173 4 00 06 52 261 0 9904 181 1 00 06 53 262 0 9904 175 5 00 06 55 263 0 9904 178 2 00 06 56 264 0 9904 177 6 00 06 58 Titration Results Method Na...

Page 18: ...18 QUICK START GUIDE QS 903 02 11 ...

Page 19: ...1 INSTRUCTION MANUAL HI 903 KARL FISCHER VOLUMETRIC TITRATOR Revision 1 00 ...

Page 20: ...the instrument This manual will provide you with the necessary information for the correct use of the instrument 2010 Hanna Instruments All rights are reserved Reproduction in whole or in part is prohibited without the written consent of the copyright owner Hanna Instruments Inc 584 Park East Drive Woonsocket Rhode Island 02895 USA ...

Page 21: ... 3 USER INTERFACE Chapter 4 GENERAL OPTIONS Chapter 5 METHODS Chapter 6 TITRATION Chapter 7 AUXILIARY FUNCTIONS Chapter 8 MAINTENANCE PERIPHERALS Chapter 9 OPTIMIZATION Appendix 1 TECHNICAL SPECIFICATIONS Appendix 2 RECOMMENDED REAGENTS Appendix 3 TITRATOR COMPONENTS ...

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Page 23: ...nd saved as a bitmap Customizable titration reports and drift analysis reports can be printed saved on a USB storage device or transferred to a PC via the USB interface Result history Titrant standardization and sample analysis results averaging GLP features Titrant age reminder Fields for specific annotations Conditioning phase Automatic pre titration for drying the solvent and titration beaker D...

Page 24: ...1 2 INTRODUCTION ...

Page 25: ...trator Left side View 2 6 2 3 4 Titrator Assembly 2 7 2 3 4 1 Connecting the Pumps 2 7 2 3 4 2 Attaching the Burette 2 9 2 3 4 3 Attaching the Beaker and Dispensing Tip 2 1 0 2 3 4 3 1 Beaker Top 2 1 1 2 3 4 4 Electrical Connections 2 1 3 2 3 5 Titrant Solvent Waste Bottle Assembly 2 1 4 2 3 5 1 Titrant Bottle Assembly 2 1 4 2 3 5 2 Solvent Waste Bottle Assembly 2 1 5 ...

Page 26: ...2 2 SETUP ...

Page 27: ...ings and Protection Tube Tube Locks Tool for Burette Cap Removal Light Protection Screen 4 Air Pump Assembly 1 pcs 5 Beaker Assembly 1 pcs Glass Beaker Beaker Ring Beaker Cap Stir Bar Desiccant Desiccant Cartridge Fittings O rings 6 Beaker Support 1 pcs 7 Pump Locking Screws with Plastic Head 2 pcs 8 Titrant Bottle Assembly 1 pcs Bottle Cap Desiccant Desiccant Cartridge Fittings O rings 9 Solvent ...

Page 28: ...tact your sales representative Note Save all packing materials until you are sure that the instrument functions correctly Any damaged or defective items must be returned in their original packing materials together with the supplied accessories 2 2 Safety Measures The following safety measures must be followed 1 Always ensure that the power supply cable is connected to a grounded main power plug 2...

Page 29: ...s Severe vibrations Direct sunlight Atmospheric relative humidity above 95 non condensing Environment temperatures below 10 C and above 40 C Explosion hazards 7 Have the titrator serviced only by qualified service personnel 2 3 Installation 2 3 1 Titrator Top View ...

Page 30: ...2 6 SETUP 2 3 2 Titrator Rear View 2 3 3 Titrator Left side View ...

Page 31: ...ect the dosing pump with the following steps see Figure 1 1 Retrieve the pump cable PUMP 1 from inside the left bay Connect the cable to the pump as shown in Figure 1 The pump connector is located in the lower part of the pump near the motor 2 Lower the pump into the titrator then slide it towards the front of the titrator chassis until it is firmly latched 3 Secure the pump with the locking screw...

Page 32: ...PUMP 2 from inside the right bay Connect the cable to the air pump as shown in Figure 2 The air pump connector is located on the left side of the motor 2 Lower the pump into the titrator then slide it towards the front of the titrator chassis until it is firmly latched 3 Secure the pump with the locking screw ...

Page 33: ...are constructed from PTFE to ensure resistance to both degradation due to Karl Fisher titrant and water vapor permeability Make sure that the mark from the valve actuating cap and the burette body are aligned as shown in Figure 3 Make sure that the valve positioning wheel on the burette pump is oriented in the proper position as shown in Figure 5 While ensuring the correct coupling between the syr...

Page 34: ...gents A sample port which can both be rapidly removed and replaced when adding solid samples and incorporates a septum through which liquid samples can be injected A desiccant cartridge containing molecular sieves and or indicating silica gel to dry the ambient air which enters the cell as solvent titrant and sample are added to or removed from the vessel Fittings made from a highly chemically res...

Page 35: ...en fittings This may cause permanent damage to o rings To assemble the 5 parts of the beaker top see Figure 7 and follow the steps below Anti Diffusion Dispensing Tip The HI903 ships with the dispensing tip A and o ring B installed For initial setup go to third step Push dispensing tip A through the dispensing tip o ring B until the o ring is at the lip of the dispensing tip Insert tip through the...

Page 36: ...ent bottle tubing or waste bottle tubing follow the steps below Loosen the 5 mm fitting H on the solvent and or waste port Remove the desired plug plugs G Insert the blue teflon tubing from the solvent and or waste bottle assemblies through the 5 mm fittings H and 5 mm o rings I until about 1 cm of tubing is visible inside the beaker Tighten the 5 mm fittings H until snug This will cause the red s...

Page 37: ... 50 60 Hz IEC Power line connector Check on titrator rear panel K C KF probe BNC socket D External magnetic stirrer 4 pin mini DIN E Connector for expansion device 8 pin DIN socket F External PC keyboard 6 pin mini DIN Standard PS2 G Analytical balance interface RS232 Standard DB 9 pin socket H PC interface USB USB socket I External display Standard VGA display 15 pin socket J Parallel Printer DB ...

Page 38: ...tle Assembly HI 900530 Caution Most Karl Fischer titrants give off harmful vapors Consult manufacturer s MSDS for safe handling guidelines To assemble the titrant bottle see Figure 9 and follow the next steps Insert teflon top J into a GL45 screw cap E Insert a desiccant cartridge B without hose barbed cap A through a 10 mm fitting F and 10 mm o ring G Insert and screw the desiccant cartridge asse...

Page 39: ... 10 mm fitting F and 10 mm o ring G Insert and screw the desiccant fitting into the corresponding hole Fasten the desiccant cartridge assembly to teflon top J with 10 mm fitting F Insert the solvent waste tube D in the 5 mm fitting H and attach the o ring I Insert and screw the tube fitting into the corresponding hole Screw GL45 E cap with full assembly onto titrant bottle Add the air tube C to th...

Page 40: ...2 16 SETUP ...

Page 41: ...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 Idle Screen 3 6 3 2 4 The Process Screen 3 7 3 3 Menu Navigation 3 8 3 3 1 Selecting an Option 3 8 3 3 2 Selecting a Menu Item 3 8 3 3 3 Entering Text 3 8 3 3 4 Saving Modifications 3 9 ...

Page 42: ...3 2 USER INTERFACE ...

Page 43: ...d by the titrator Turn on the titrator using 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 using the power switch If t...

Page 44: ...Function Keys If one of these keys is pressed the associated function is immediately performed Some of the keys are only active in specific screens Starts or stops titration sequence Turns the stirrer ON and OFF Idle mode only 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 bo...

Page 45: ...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 Accepts alphanumeric data entry Executes the default underlined virtual option key 3 2 2 Display The titrator has a large color graphical display The standby mode screen is shown below with short explanations of the sc...

Page 46: ...Displays the current date and time Stirrer information Actual Set stirrer speed is displayed in RPM When stirrer is off the stirrer information is not displayed Titrant Displays the name of the current titrant Last Standardization Displays the titrant standardization date time Reminders Indicates when a task needs to be performed and displays error or warning messages Idle Screen fields ...

Page 47: ...t Standardization Process status Displays the process status with a descriptive drawing mV reading Displays the KF electrode potential Dispensed titrant Displays the total volume of dispensed titrant Last dose Displays the last titrant dose volume Drift value Displays the drift value when available Stirrer information Actual Set stirrer speed is displayed in RPM Burette status A descriptive drawin...

Page 48: ...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 me...

Page 49: ...ing 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 press again to return to the previous screen ...

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Page 51: ...uage 4 6 4 6 Estimated Cell Volume 4 6 4 7 Titrant Database 4 6 4 8 Standard Database 4 7 4 9 Save Files to USB Storage Device 4 7 4 10 Restore Files from USB Storage Device 4 9 4 11 USB Link with PC 4 1 0 4 12 Calibration Check 4 1 0 4 13 Setup Balance Interface 4 1 1 4 14 Printer Mode 4 1 2 4 15 Reset to Default Settings 4 1 3 4 16 Update Software 4 1 3 ...

Page 52: ...4 2 GENERAL OPTIONS ...

Page 53: ... Press or to change the time format 4 GENERAL OPTIONS The General Options screen gives access to options that are not directly related to the titration process To access this screen press from the main screen while in idle mode In Pre titration Drift Analysis Standby or Titration process the General Options can be accessed by pressing the Home key on a PS 2 keyboard The available menus are describ...

Page 54: ...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 backlight is off any keystroke will re activate the backlight without performing any action The range for backlight saver interval is between 1 and 60 minutes To disable the backlight saver increase the time to the maximum allowed...

Page 55: ...when a critical error occurs during titration 4 4 Stirrer This screen allows the user to select the internal magnetic stirrer an external magnetic stirrer or a user controlled stirrer uncontrolled by the titrator custom The external stirrer is automatically detected when it is connected Note When the external stirrer is not connected the key is not available for the External stirrer option ...

Page 56: ...ion in the titration beaker 4 7 Titrant Database This screen allows the user to store information about all of the titrants available for use including the titrant name and Standardization information The titrant for the currently selected method cannot be modified from this screen For details on the full functionality of the database see section 5 5 12 ...

Page 57: ... from this screen For details on the full functionality of the database see section 5 5 11 4 9 Save Files to USB Storage Device This option allows the user to save files from titrator to a USB storage device On the titrator the available file types are Standard Method Files HIxxxxyy MTD e g HI8001EN MTD HI8101EN MTD User Method Files USERxxxx MTD e g USER0001 MTD Drift Titration Report Files DR_xx...

Page 58: ...ice Deletes the highlighted file Deletes all currently displayed files 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 HI 903 folder as follows Methods USB Drive HI 903 Methods mtd Reports USB Drive HI 903 Reports rpt Insert the USB Storage Device ...

Page 59: ...he and keys to scroll through the list The number of files and the name of each file found on the USB storage device is displayed on the screen The option keys allow the following operations Returns to the General Options screen Copies the highlighted file from the USB storage device to titrator Copies all currently displayed files from the USB storage device to titrator Deletes the highlighted fi...

Page 60: ...r is not connected to the HI 900 PC Application Active The titrator is connected to the HI 900 PC Application Ready The titrator is ready for commands Transmit It shows the progress of the current transfer Speed It shows the baud rate for the communications port 4 12 Calibration Check This screen allows the user to verify the analog board calibration Two parameters can be verified the electrode mV...

Page 61: ...meter to µA mode If necessary switch the calibration key to µA mode by pressing the red button Connect the calibration key banana plugs to the multimeter mA input Check for the multimeter indication to be in accordance with the titrator µA prescribed value 4 13 Setup Balance Interface This screen allows the user to setup an analytical balance for automatic acquisition of sample mass prior to titra...

Page 62: ...ection with the balance is working properly by pressing the key 4 14 Printer mode This screen allows the user to select the printing mode ANSI default ASCII and Text mode ANSI mode Use this mode when your printer is set to ANSI In this case all accepted characters symbols available on the titrator will be printed by your printer ASCII mode Use this mode when your printer is set to ASCII In this ca...

Page 63: ...e be careful This will also delete all the user created methods reports and restore all manufacturer settings such as titrator configuration standard method parameters etc 4 16 Update Software This screen allows the user to update the titrator software from a USB storage device con taining a software setup kit ...

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Page 65: ... 5 6 5 5 Method Options 5 7 5 5 1 Naming the User Method 5 7 5 5 2 Method Revision 5 8 5 5 3 Method Type 5 8 5 5 4 Predispensing Amount 5 9 5 5 5 Pre Analysis Stir Time 5 9 5 5 6 Stirring Speed 5 10 5 5 7 Stirbar Type 5 10 5 5 8 Drift Entry 5 11 5 5 9 Solvent Name 5 12 5 5 10 Sample Parameters Sample Analysis mode only 5 12 5 5 10 1 Sample Determination 5 13 5 5 10 2 Sample Name 5 13 5 5 10 3 Samp...

Page 66: ...5 13 Control Parameters 5 19 5 5 13 1 Start Mode 5 19 5 5 13 2 Standby Mode 5 20 5 5 13 3 Standby Duration 5 20 5 5 13 4 Imposed Current 5 21 5 5 13 5 Dosing Parameters 5 21 5 5 13 6 Timed Increment 5 22 5 5 13 7 End Point Value 5 22 5 5 13 8 Signal Averaging 5 23 5 5 13 9 Flow Rate 5 23 5 5 14 Termination Parameters 5 24 5 5 14 1 Maximum Duration 5 24 5 5 14 2 Maximum Titrant Volume 5 25 5 5 14 3...

Page 67: ...ed on the screen 5 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 Standard and user methods can be upgraded stored or deleted by connecting the titrator to a PC using the HI900PC application or a USB storage device 5 1 Selecting Methods To select a method press the key when available A list of availa...

Page 68: ...vice will be displayed Press the or key to upgrade the titrator with the standard methods Press to return to General Options screen Note See section 4 8 Restore Files from USB Storage Device From PC You can upgrade the titrator with standard methods from a PC using the HI 900 PC applica tion see Section 4 9 USB Link with PC 5 2 2 Deleting Standard Methods Unnecessary standard methods can be remove...

Page 69: ...difying 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 methods list Press A new user method will ...

Page 70: ... modify and choose Note Only a limited number of user methods can be generated 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 when available 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 p...

Page 71: ...fications press and select Save Method to keep the changes 5 5 Method Options 5 5 1 Naming the User Method This option allows you to enter a 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 ...

Page 72: ...r has to choose between water determination in the sample Sample Analysis or determination of titrant concentration Titrant Standardization 5 5 2 Method Revision This option allows you to enter a string representing the current method revision The revision string format should be X Y where X and Y are numerical digits ...

Page 73: ...etting the amount to 0 will disable the titrant predispensing feature 5 5 5 Pre Analysis Stir Time To avoid erroneous results or unreacheable endpoints when analyzing samples with limited solubility the sample must be completely dissolved in the solvent prior to the start of a titration The pre analysis stir time can be set between 0 and 1000 seconds After the sample is added to the reaction vesse...

Page 74: ...etween 200 and 2000 RPM with a resolution of 100 RPM The stirrer will remain on as long as the method is active The speed can be adjusted at any time by using the and keys when the stirrer is running 5 5 7 Stirbar Type Allows the user to edit the stirbar description ...

Page 75: ...ess Automatic the drift rate will be calculated automatically after the Pre titration of the solvent User the drift is set to a fixed value entered by the user The user enters the estimated drift value The drift analysis stage will be skipped and the user must enter the drift value between 0 0 µg min and 10 0 µg min ...

Page 76: ...t up to 15 characters Use the arrow keys to navigate through the character table Press to add the highlighted character to the solvent name 5 5 10 Sample Parameters Sample Analysis mode only This screen allows the user to access and configure the specific sample parameters ...

Page 77: ... from which the water is extracted and released into the solvent External dissolution is a method for the preparation of the following types of samples samples with a very high water content samples that do not exhibit a homogeneous water distribution slow dissolving samples samples that can contaminate the titration vessel thus reducing the accuracy precision num ber of titrations between solvent...

Page 78: ...rior to analysis 5 5 10 4 Sample Size This option allows the user to enter the sample size For external Dissolution enter the size of the aliquot taken from the external vessel Before the titration is started the user is asked again to enter the sample size The sample size mass or volume can be automatically acquired from the balance when the balance feature is enabled see Section 4 11 Setup Balan...

Page 79: ...ly Enter the amount of sample added to the External Dissolution vessel 5 5 11 Standard Titrant Standardization mode only This screen allows the user to define a list of Karl Fischer standards and customize related parameters Using the and keys highlight the standard from the existing list and press to choose it Press New Standard if you want to create and add a new standard to the Karl Fischer sta...

Page 80: ... 5 11 4 Water Content The concentration of the standard can be entered content of water in the selected unit 5 5 12 Standard Size Enter the amount of standard used during titrant standardization Before the titrant standardization is started the user is asked again to enter the standard size The standard size mass and volume can be acquired automatically from a compatible analytical balance when th...

Page 81: ...hoose it Press New Titrant to create a new titrant Press to remove the titrant from the list Press Edit to edit the titrant parameters Hanna Standard Methods are designed to be used with titrants of specific types and concen trations The HI903 will automatically select an appropriate titrant when such a method is selected If there is no usable titrant in the database a new one will be created ...

Page 82: ...or the titrant 5 5 13 2 Titrant Type The user can select the type of titrant 5 5 13 3 Nominal Titrant Concentration The user can enter the titrant concentration 5 5 13 4 Standardized Titrant Concentration The user can manually enter the exact titrant concentration ...

Page 83: ...ncentration is necessary When the set reminder period has expired a warning message will be displayed on the main screen The reminder period will reset once the titrant is restandardized or the set time is modified 5 5 14 Control Parameters The user can access and edit the parameters related to the titration ...

Page 84: ...der to prevent over titration In Normal mode the titrant dosing begins with the median value between the minimum and maximum i e minimum dose 5 µL maximum dose 25 µL first dose will be 15 µL 5 5 14 2 Standby Mode When enabling this option the titrator will automatically revert to Standby mode after a titration is completed See also the Standby Duration option ...

Page 85: ... and 59 minutes 5 5 14 4 Imposed Current The HI 903 uses a bivoltametric electrode system During a titration the titrator monitors the voltage required to maintain a constant polarization current imposed current This option allows the user to select the electrode polarization current from the predefined list Note Higher polarization currents will speed the contamination of the electrode and potent...

Page 86: ...gent reagent concentra tion and the expected content of water in the sample Correct determination of these values is necessary in order to prevent over titration and ensure the highest possible accuracy 5 5 14 6 Timed Increment The user can enter the period of time between two successive doses The time period must be defined in accordance with the specifics of the analysis ...

Page 87: ...me The mV value can be set from 5 0 to 600 0 mV 5 5 14 8 Signal Averaging This option enables averaging of the mV reading when enabled If 1 Reading is selected the filtering is disabled The titrator will take the last reading and places 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...

Page 88: ...he burette volume 0 1 to 10 mL min for a 5 mL burette Note The titrator will automatically detect the burette size and display the correct high limit volume The flow rate is set for all burette operations 5 5 15 Termination Parameters This screen allows the user to set the control parameters related to the end of the titration ...

Page 89: ...n will be terminated after the maximum titrant volume has been dispensed The error message Limits Exceeded will appear on the display Range is from 0 100 to 50 000 mL 5 5 15 1 Maximum Duration Specify the maximum time a titration is allowed to run Once this point is reached the titration will be terminated even if the end point is not reached The time can be set from 10 to 3600 seconds ...

Page 90: ...y Time Absolute Drift The titration is terminated when the actual drift is less than the pre defined absolute drift value Relative Drift The titration is terminated when the actual drift is less than the sum between the initial drift and the predefined relative drift 5 5 15 4 End Point Stability Time This screen allows users to set the time period in which the electrode potential must remain stabl...

Page 91: ... 5 6 Printing To print method parameters press from the main screen then If no printer is connected to the dedicated socket or if the printer is offline an error message will appear on the display see Section 8 3 3 Connecting a Printer for information about connecting a printer to the titrator ...

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Page 93: ...ITRA TITRA TITRA TITRATION TION TION TION TION Chapter 6 Contents 6 TITRATION 6 3 6 1 Idle 6 3 6 2 Pre titration 6 3 6 3 Drift Analysis 6 4 6 4 Standby 6 5 6 5 Sample Analysis 6 6 6 6 Titrant Standardization 6 11 ...

Page 94: ...6 2 TITRA TITRA TITRA TITRA TITRATION TION TION TION TION ...

Page 95: ...g solvent system are properly assembled The right amount of solvent is present in the beaker between the min and max marks for best reproducibility The following intermediary stages are performed automatically before starting the analysis Solvent pre titration Drift analysis Automatic Drift Entry only When the drift analysis process is finished the titrator enters Standby mode At this point a titr...

Page 96: ... as the background drift rate or the drift rate The drift rate is determined by keeping track of the number of very small successive doses of titrant required to maintain the dryness of the solvent over the course of a minute The rate at which water leaks into the cell is then calculated and reported by the HI 903 in units of µg min The HI 903 uses the drift rate determined during this state to au...

Page 97: ... and general options external keyboard only by pressing Home After an initial titrator setup and prior to the first titration or standardization the drift rate should be allowed to settle in Standby mode for 45 min This ensures that the drift rate is stable and reflects the actual rate at which water vapor is entering the cell rather than representing a slow drying of the air between the solvent a...

Page 98: ... by pressing or to return to Standby mode by pressing in order to wait until the drift is stabilized at a higher value Entering estimated concentration The user has the option to enter the estimated con centration which is in accordance with the pre titration amount and the suggested optimal limits Adding the sample The user must add the sample into the titration vessel via the sample port Enterin...

Page 99: ...mple volume 2 Rinse the syringe and needle with sample several times by drawing in a small portion of sample fully extending the plunger shaking to coat the syringe interior and expelling the sample into a waste collection container 3 Draw enough sample into the syringe for at least one titration 4 Dry the outside of the needle with a lint free wipe or tissue 5 Insert the needle through the septum...

Page 100: ... the RS232 interface Note The user must make sure that the balance and the titrator are properly configured and the balance feature is enabled see Section 4 10 Setup Balance Interface Procedure 1 Place the syringe or the weighing boat containing the sample on the balance 2 Wait until the reading is stabilized and press 3 Add the sample in the titrator vessel 4 Place the empty syringe or weighing b...

Page 101: ...ous screen and the sample size is automatically updated Now the analysis can be started Start Analysis Press to begin analysis Suspend Titration While the titration is in progress you can temporarily stop it by pressing The burette will stop dispensing titrant To continue the titration press ...

Page 102: ... the titration manually and return to Idle mode Press to stop the titration and return to Standby mode When the end point is reached the titration is finished and the following screen is displayed This screen displays information about the titration duration drift value used for compensa tion sample size titrant concentration dispensed titrant volume titration report ID Press to see the titration ...

Page 103: ...eys to scroll the concentration results list Use to choose the sample concentration results that will be used for averaging Note When there are no results selected dashes will appear in the Average Sample Concen tration and the Standard Deviation fields 6 6 Titrant Standardization While in Standby mode press Note If the drift value is zero a warning message appears to inform the user that the solv...

Page 104: ...g samples see Section 6 5 Sample Analysis Start Standardization Press to begin standardization Note During titrant standardization the user has the same options as a sample analysis see Section 6 5 Sample Analysis When the titrant standardization is finished the user has two options to update the titrant concentration By pressing the titrant is updated with the current result By pressing the user ...

Page 105: ...verage of titrant concentration Use the and keys to scroll the concentration results list Use to choose the titrant concentration results that will be used for averaging Press to update the concentration with the current average Note When there are no results selected dashes will appear in the average titrant concentra tion and the standard deviation fields is not available in this case ...

Page 106: ...6 14 TITRA TITRA TITRA TITRA TITRATION TION TION TION TION ...

Page 107: ...p 7 3 7 1 1 Filling the Beaker 7 3 7 1 2 Emptying the Beaker 7 3 7 2 Burette 7 4 7 2 1 Prime Burette 7 4 7 2 2 Rinse Tip 7 5 7 2 3 Manual Dispense 7 5 7 2 4 Purge Burette 7 6 7 3 Stirrer 7 6 7 4 Results 7 7 7 4 1 Review Last Titration Report 7 7 7 4 2 Review Available Reports 7 8 7 4 3 GLP Data 7 8 7 4 4 Meter Information 7 9 7 4 7 Setup Titration Report 7 1 0 ...

Page 108: ...7 2 AUXILIARY FUNCTIONS AUXILIARY FUNCTIONS AUXILIARY FUNCTIONS AUXILIARY FUNCTIONS AUXILIARY FUNCTIONS ...

Page 109: ...dicator line If the solvent is not flowing or is flowing very slowly verify that the bottle top assemblies are properly assembled and tightly sealed and that the liquid handling tubing reaches the bottom of the solvent bottle 2 When the level of solvent inside the titration cell reaches the min line release the Fill button and deactivate the air pump with the option key 3 The HI 903 will prompt th...

Page 110: ...components 7 2 1 Prime Burette After solvent has been added to the titration cell the burette can be primed with titrant The priming process consists of several cycles of filling and emptying the burette with titrant It ensures that any air water or water vapor in the burette or tubing is removed Two rinse cycles of burette are shown in the figure below The dispensing tube is connected on the righ...

Page 111: ...ssure that the air bubbles are completely removed 7 2 2 Rinse Tip A 0 25 mL dose of titrant will be dispensed from the burette when this operation is selected This operation will eliminate any contamination from the anti diffusion dispensing tip 7 2 3 Manual Dispense Manual Dispense allows a defined titrant volume to be be dosed Select the Manual Dispense option and press The Manual Volume Dispens...

Page 112: ...on tube from the titrant bottle The figures below show the steps in a purge burette operation 7 3 Stirrer Note When custom stirrer is selected see Section 4 4 Stirrer in General Options chapter the commands related to the stirrer are not available The stirrer can be turned on and off by pressing while in Idle mode During the titration process the stirrer cannot be turned off The stirring speed is ...

Page 113: ...a Parameters screen you can access the following options 7 4 1 Review Last Titration Report The last titration report can be reviewed The titration graph can be reviewed by selecting The information seen in the report is based on the selections made in the Setup Titration Report screen The following option keys are available Review the titration graph Print the titration report ...

Page 114: ...press Report All of the saved reports can be reviewed and printed The report contains only the information selected in the Setup Titration Report screens during report generation The following option keys are available Review the titration graph Print the titration report Delete the selected report 7 4 3 GLP Data GLP data can be optionally be displayed in each report Enter up to 20 alphanumeric ch...

Page 115: ...ation Displays titrator configuration data Titrator Serial Number The serial number of the titrator base board Analog Board Serial Number The serial number of the titrator analog board Dosing Pump Serial Number The serial number of the connected pump Titrator Software Version The current software version installed on the titrator Base Board Software Version The current software version present on ...

Page 116: ...ILIARY FUNCTIONS AUXILIARY FUNCTIONS AUXILIARY FUNCTIONS AUXILIARY FUNCTIONS 7 4 5 Setup Titration Report Customize a unique report to record the titration results An asterisk means that it will be included in the titration report ...

Page 117: ...ube and Aspiration Tube 8 4 8 1 4 Assembling the Dispensing Tube and Aspiration Tube 8 4 8 1 5 Cleaning the Burette 8 5 8 1 6 Burette Preparation Filling with Titrant 8 7 8 2 Probe Maintenance 8 8 8 3 Fuse Replacement 8 9 8 4 Peripherals 8 9 8 4 1 Connecting an External Display 8 1 0 8 4 2 Connecting an External PC Keyboard 8 1 0 8 4 3 Connecting a Printer 8 1 2 8 4 4 Connecting to a Computer 8 1 ...

Page 118: ...8 2 MAINTENANCE PERIPHERALS ...

Page 119: ...es mounted see Section 2 3 4 2 Attaching the Burette for assembly details The burette assembly consists of a rigid housing which holds the glass syringe a 3 way valve and is connected to titrant tubing with specially designed fittings Note The dispensing tube has two fitted ends One end is equipped with a burette fitting and the other is equipped with a beaker fitting 8 1 2 Changing the Burette Re...

Page 120: ...the burette holder Unscrew the fitting C Repeat these steps for the aspiration tube 8 1 4 Assembling the Dispensing Tube and Aspiration Tube To attach the dispensing tube and the aspiration tube follow these steps Insert the end of the dispensing tube with the tan colored fitting A into the valve outlet Screw in the fitting so that the highest of its 9 cuts stays vertical in the final posi tion Be...

Page 121: ... from the solvent or cleaning solution 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...

Page 122: ...th bare hands or greasy materials Consult Manufacturer s MSDS for safe handling instructions 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 Position the piston shaft to couple the pump correct...

Page 123: ...e burette needs to be rinsed minimum three rinses are recommended allowing air bubbles to be evacuated Press Insert the aspiration tube into the titrant bottle only when the piston is going down and has reached about from the top To avoid the presence of air bubbles inside the burette make sure to have continuous liquid flow inside the burette and a little air just above the liquid level during th...

Page 124: ... electrode with a solvent that is appropriate for the type of sample used methanol is usually sufficient Allow the probe to dry completely before re installing If a more thorough cleaning is required soak the electrode in HI 7061 Electrode Cleaning Solution for General Use for several hours then rinse with water followed by methanol Allow to dry before re installing After allowing the probe to dry...

Page 125: ...uses see the label located above the main power switch Close the fuse holder cover Connect the power cord Note For other maintenance operations please contact your dealer or the nearest Hanna Customer Service Center 8 4 Peripherals Warning Connection disconnection of POWER CORD PUMP ASSEMBLY EXTERNAL PC DISPLAY PRINTER RS232 INTERFACE or EXPANSION DEVICE must be done only when titrator and externa...

Page 126: ...VGA display connected 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 8 4 2 Connecting an External PC Keyboard This connection allows you to use an external PS 2 PC Keyboard in addition to titrator s keypad Connect an external PC Keyboard PS 2 connector ...

Page 127: ...n 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 Home access General Options Alphanumeric Keys Allow alphanumeric entries ...

Page 128: ... printer 8 4 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 Connect the cable to the USB port on the rear panel of the titrator Connect the cable to the USB port on the PC Select the USB Link with PC screen on the titrator by following the path General Options USB Link with PC Launch the HI 900 PC appli...

Page 129: ...9 1 1 5 Signal Averaging 9 6 9 1 1 6 Flow Rate 9 6 9 1 2 Termination Parameters 9 6 9 1 2 1 Stability Time 9 6 9 1 2 2 Drift Stop Termination Criteria 9 6 9 1 2 2 1 Relative Drift Stop 9 7 9 1 2 2 2 Absolute Drift Stop 9 7 9 1 3 Method Options 9 8 9 1 3 1 Pre Dispensing Amount 9 8 9 1 3 2 Pre Analysis Stir Time 9 8 9 1 3 3 Stirring Speed 9 8 9 1 3 4 Background Drift Rate Entry 9 8 9 2 The Sample 9...

Page 130: ...ernal Extractions 9 1 3 9 2 5 5 Homogenization 9 1 4 9 2 5 6 Heating 9 1 4 9 3 Karl Fischer Reagent System 9 15 9 3 1 Reagent System Classification 9 1 5 9 3 1 1 One Component Reagent Systems 9 1 5 9 3 1 2 Two Component Reagent Systems 9 1 5 9 3 1 3 Reagents for Aldehydes and Ketones 9 1 5 9 3 2 Choosing and Modifying a Solvent 9 1 6 9 3 3 Water Standards 9 1 6 9 3 4 Standardizing the Titrant 9 1 ...

Page 131: ...n During a titration no excess iodine is present In order to maintain the set polarization current the HI 903 must apply a relatively large voltage across the pins of the electrode At the endpoint of the titration the amount of iodine added is equal to the amount of water from the sample When an excess of titrant has been added iodine is present in the solution The excess iodine is easily reduced ...

Page 132: ...t determination and faster titrations The minimum and maximum dose volume must be set appropriately by the user for dynamic dosing to be effective 9 1 1 2 1 Minimum Dose Decreasing the minimum dose increases precision but lengthens the titration time The only exception is when stability time has been selected as the termination criteria and there is a high drift rate Under these circumstances the ...

Page 133: ...rement This setting controls the amount of time between successive titrant doses Setting the time increment appropriately is important to ensure that the titrant has adequate time to mix with the sample such that the electrode measures a homogeneous solution before the titrator makes the decision on the size of the next dose of titrant The value of the timed increment is dependent on the type of r...

Page 134: ...mination criteria is selected a titration is considered to have reached an endpoint when the electrode potential stays below the specified endpoint potential for a period of time called the stability time Typical endpoint stability times range between 5 and 15 seconds In order for this criteria to successfully terminate a titration the stability time and the minimum dose size must be set such that...

Page 135: ...cern when using reagents that have slower reaction rates one component or aldehyde and ketone reagents It is important to set an appropriate relative drift stop value when working with insoluble or sparingly soluble samples During these types of titrations the final traces of water are released very slowly If the sample contains a small amount of water the final traces are a large fraction of the ...

Page 136: ... stirring system is equipped with an optical feedback mechanism to ensure that the stirring motor is rotating at the speed set by the user The optimum stirring speed is obtained when a small vortex is visible If the stirring speed is too low the titrant will not react with the sample before reaching the electrode resulting in over titration and poor titration reproducibility If the stirring speed ...

Page 137: ...lk materials Surfaces of hygroscopic materials may contain higher levels of moisture relative to the rest of the material Surfaces of materials which release water may contain less water relative to the rest of the material 4 Taking large samples of bulk materials will result in a more representative sample 9 2 2 Determining the Optimal Sample Size The proper choice of sample size is critical to a...

Page 138: ...or solvent mixture dissolution of a solid sample can be aided by grinding the sample into a fine powder increasing the pre analysis stir time or heating the solvent during a titration with an optional jacketed titration cell and water circulator Solid samples are added to the titration cell by removing the sample plug The quantity of solid sample added can be entered into the HI 903 as a mass or b...

Page 139: ...3 Draw enough sample into the syringe for at least one titration 4 Dry the outside of the needle with a lint free wipe or tissue 5 Determine the mass of the syringe and sample 6 Initiate a titration from standby mode by pressing the start analysis option key 7 Insert the needle through the septum in the sample port Push the syringe through the septum until the end of the needle is approximately 1 ...

Page 140: ...ssolution 9 2 5 1 Internal Extractions Internal extractions are carried out using the normal sample type option within the sample parameters menu This type of sample preparation is suitable for solid samples which release their water relatively quickly during the pre analysis stir time and exhibit limited or no solubility in Karl Fischer solvents Internal extraction should be used preferentially o...

Page 141: ...vely small amount of solvent A small portion of the solvent can then be injected into the titration vessel Sample preparation and choice of solvent or solvent mixture is sample specific Consult an applicable standard method for procedural details The HI 903 will conduct the necessary calculations automatically when external dissolution is selected from the sample type menu 9 2 5 4 External Extract...

Page 142: ...distributions and must therefore be thoroughly reduced to powder or homogenized The procedure for homogenization depends upon the characteristics of the specific sample Homogenization is particularly suited for semi solid samples and suspensions and is the only method that can disrupt plant and tissue cells in order to release water present inside the cells Homogenization is typically carried out ...

Page 143: ... with respect to the chemical composition of the solvent and provides a nearly limitless solvent capacity for water One component solvent systems can be easily customized creating mixtures specially adapted to specific sample characteristics without having to worry about providing appropriate levels of sulfur dioxide and buffer components Common solvent mixtures include ethanol chloroform xylene t...

Page 144: ...thanol Co solvents of long chain alcohols n decanol or chloroform should used Carbohydrates and proteins have poor solubility in methanol formamide can be used as a co solvent Analyzing acids or bases may take the pH outside the optimal range and additional buffering may be required a commercial Karl Fischer Buffer reagent can be added or extra imidazole can be added for acid samples and salicylic...

Page 145: ...e analyses 2 Select the appropriate standardization method included with the HI 903 Using a Sodium Tartrate Dihydrate Standard 3 Back weigh between 30 and 200 mg of standard Be sure that the salt is a high quality standard which has been stored properly and exists as a fine free flowing powder 4 Repeat the standardization at least three times and update the titrant concentration using the averaged...

Page 146: ...ATION 5 Review the set of results on the average results statistics screen The titrant concentration should be updated with the averaged results as long as there is not excessive variability between standardization results ...

Page 147: ...A1 1 APPENDIX 1 Appendix 1 Contents A1 TECHNICAL SPECIFICATIONS A1 3 ...

Page 148: ...A1 2 APPENDIX 1 ...

Page 149: ...L precision ground with PTFE plunger Valve Motor driven 3 way PTFE liquid contact material Tubing PTFE with light block and thermal jacketing Dispensing Tip Glass fixed position anti diffusion Titration Vessel Conical with operating volume between 50 150 mL Solvent Handing System Sealed system integrated diaphragm air pump Electrode Type Dual platinum pin polarization electrode Connection BNC Pola...

Page 150: ... 5 7 320 x 240 Pixel Color LCD Power Supply HI 903 01 115 VAC 50 60 Hz HI 903 02 230 VAC 50 60 Hz Power Draw HI 903 01 0 2 Amps HI 903 02 0 1 Amps Fuses 2 Exchangeable Fuses Languages English Portuguese Spanish Titration Methods Up to 100 standard and user methods Data Storage Up to 100 complete titration reports and drift rate reports can be stored GLP Conformity Good Laboratory Practice and Inst...

Page 151: ...ded Reagents A2 RECOMMENDED REAGENTS A2 3 A2 1 Titrants A2 3 A2 1 1 1 component Titrants A 2 3 A2 1 2 2 component Titrants A 2 3 A2 2 Solvents A 2 3 A2 2 1 1 component Solvents A 2 3 A2 2 2 1 component Solvents A 2 4 A2 3 Standards A2 4 ...

Page 152: ......

Page 153: ...rich 34723 HYDRANAL Titrant 2E 34811 HYDRANAL Titrant 2 GFS Chemicals 1603 WaterMark Stable 2 mg mL Non hygroscopic 1604 WaterMark Stable 5 mg mL Non hygroscopic 1616 WaterMark 5 mg mL in Methanol 1970 WaterMark Stable 0 5 mg mL Non hygroscopic J T Baker 8844 HYDRA POINT Titrant 5 8845 HYDRA POINT Titrant 2 A2 2 Solvents A2 2 1 1 component Solvents Sigma Aldrich 34697 HYDRANAL Solver Crude Oil Wor...

Page 154: ... WaterMark Solvent General Purpose J T Baker 8855 HYDRA POINT Solvent G A2 3 Standards Sigma Aldrich 34803 HYDRANAL Standard Sodium Tartrate Dihydrate 34828 HYDRANAL Water Standard 1 00 34847 HYDRANAL Water Standard 0 10 34849 HYDRANAL Water Standard 10 0 GFS Chemicals 2302 KF Water Standard 1 0 mg g ...

Page 155: ...A3 1 APPENDIX 3 Appendix 3 Accesories A3 TITRATOR COMPONENTS A3 3 ...

Page 156: ......

Page 157: ...Beaker for HI903 HI900523 Dispensing tip 2pcs HI900527 Septum 5pcs HI900528 Solvent Port Plugs 2pcs HI900530 Titrant Bottle Top Assembly HI900531 Solvent WasteBottleTop Assembly HI900532 Desiccant Cartridge for Beaker or Titrant A3 TITRATOR COMPONENTS ...

Page 158: ...x Tubing for Air Pump HI900540 O Ring Set HI900570 Aspiration Tubing HI900580 Dispensing Tubing and fitting HI900550 Desiccant 250 g HI900810 Manual English for HI 903 HI900903U PC Application on USB Flash Drive HI900941 Calibration Key HI900942 Tool for Burette Cap Removal HI900943 Fuses 1A UL x 2 pcs HI900944 Fuses 2A UL x 2 pcs MAN HI903 05 12 ...

Page 159: ...1 GENERAL APPLICATIONS BROCHURE HI 903 KARL FISCHER VOLUMETRIC TITRATOR Revision 1 00 ...

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Page 162: ...1 0 Results Titration Report Method Name Stdz 5mg mL w water Std Time Date 12 00 Jan 1 2011 Standard Size 1 0000 g Standard Conc 10 0000 mg g Drift Value 5 4 ug min End Point Volume 2 0341 mL Result 4 9276 mg mL Titration Duration 4 19 mm ss Estimated Cell Volume 55 88 mL Titration went to Completion Operator Name Analyst Signature ________________________ ...

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Page 164: ...1 0 Results Titration Report Method Name Stdz 2mg mL w water Std Time Date 12 00 Jan 1 2011 Standard Size 2 0000 g Standard Conc 1 0000 mg g Drift Value 5 0 ug min End Point Volume 1 0605 mL Result 1 9103 mg mL Titration Duration 5 10 mm ss Estimated Cell Volume 60 11 mL Titration went to Completion Operator Name Analyst Signature ________________________ ...

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Page 166: ...1 0 Results Titration Report Method Name Stdz 1mg mL w water Std Time Date 12 00 Jan 1 2011 Standard Size 2 0000 g Standard Conc 1 0000 mg g Drift Value 5 0 ug min End Point Volume 1 8732 mL Result 1 0824 mg mL Titration Duration 5 30 mm ss Estimated Cell Volume 64 20 mL Titration went to Completion Operator Name Analyst Signature ________________________ ...

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Page 168: ...ods r 1 0 Results Titration Report Method Name Stdz 5mg mL w Tartrate Time Date 12 00 Jan 1 2011 Standard Size 0 1000 g Standard Conc 15 66 Drift Value 4 0 ug min End Point Volume 3 1185 mL Result 5 0329 mg mL Titration Duration 8 48 mm ss Estimated Cell Volume 69 26 mL Titration went to Completion Operator Name Analyst Signature ________________________ ...

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Page 170: ...ort Method Name Moisture in Dairy Cream Time Date 12 00 Jan 01 2011 Sample Size 0 0241 g Std Titrant Conc 5 0000 mg mL Drift Value 4 7 ug min End Point Volume 3 4567 mL Result 71 5481 Titration Duration 8 36 mm ss Estimated Cell Volume 65 72 mL Titration went to Completion Operator Name Analyst Signature ________________________ ...

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Page 172: ...ort Method Name Moisture in Milk Time Date 12 00 Jan 01 2011 Sample Size 0 0188 g Std Titrant Conc 5 0000 mg mL Drift Value 4 5 ug min End Point Volume 3 2614 mL Result 86 5886 Titration Duration 6 18 mm ss Estimated Cell Volume 60 03 mL Titration went to Completion Operator Name Analyst Signature ________________________ ...

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Page 176: ...on Report Method Name Surface Moisture Sugar Time Date 12 00 Jan 1 2011 Sample Size 7 5231 g Std Titrant Conc 1 0000 mg mL Drift Value 5 7 ug min End Point Volume 2 4292 mL Result 319 ppm Titration Duration 4 42 mm ss Estimated Cell Volume 62 4 mL Titration went to Completion Operator Name Analyst Signature ________________________ ...

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Page 178: ...port Method Name Moisture in Cooking Oil Time Date 12 00 Jan 1 2011 Sample Size 4 0296 g Std Titrant Conc 1 0000 mg mL Drift Value 3 4 ug min End Point Volume 2 6808 mL Result 660 ppm Titration Duration 6 30 mm ss Estimated Cell Volume 58 11 mL Titration went to Completion Operator Name Analyst Signature ________________________ ...

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Page 180: ... Imposed Current 20 uA Minimum Dose 0 5000 uL Maximum Dose 40 0000 uL Timed Increment 1 second End Point Value 180 0 mV Signal Averaging 3 Readings Flow Rate 10 0 mL min Termination Parameters Maximum Duration 720 sec Maximum Titrant Volume 10 0000 mL Term Criterion Relative Drift Relative Drift 15 0 ug min Result Unit Calculations Titrant units mg mL Titrant volume consumed V mL Final results uni...

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Page 182: ...es Imposed Current 20 uA Minimum Dose 1 0000 uL Maximum Dose 50 0000 uL Timed Increment 1 second End Point Value 180 0 mV Signal Averaging 3 Readings Flow Rate 10 0 mL min Termination Parameters Maximum Duration 720 sec Maximum Titrant Volume 10 0000 mL Term Criterion Relative Drift Relative Drift 15 0 ug min Result Unit Calculations Titrant units mg mL Titrant volume consumed V mL Final results u...

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Page 184: ...nutes Imposed Current 20 uA Minimum Dose 0 5000 uL Maximum Dose 20 0000 uL Timed Increment 1 second End Point Value 180 0 mV Signal Averaging 3 Readings Flow Rate 10 0 mL min Termination Parameters Maximum Duration 720 sec Maximum Titrant Volume 10 0000 mL Term Criterion Relative Drift Relative Drift 10 0 ug min Result Unit Calculations Titrant units mg mL Titrant volume consumed V mL Final result...

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Page 186: ...ort Method Name Moisture in Shampoo Time Date 12 00 Jan 1 2011 Sample Size 0 0200 g Std Titrant Conc 5 0000 mg mL Drift Value 5 4 ug min End Point Volume 3 2010 mL Result 79 9207 Titration Duration 7 19 mm ss Estimated Cell Volume 106 37 mL Titration went to Completion Operator Name Analyst Signature ________________________ ...

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Page 188: ...eport Method Name Moisture Hand Cream Time Date 12 00 Jan 1 2011 Sample Size 0 0244 g Std Titrant Conc 5 0000 mg mL Drift Value 5 4 ug min End Point Volume 2 6925 mL Result 67 3125 Titration Duration 6 48 mm ss Estimated Cell Volume 106 37 mL Titration went to Completion Operator Name Analyst Signature ________________________ ...

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Page 190: ...ethods r 1 0 Results Titration Report Method Name Solvent w 5mg mL 1 comp Time Date 12 00 Jan 01 2011 Sample Size 0 9580 g Std Titrant Conc 5 0000 mg mL Drift Value 4 0 ug min End Point Volume 0 1157 mL Result 0 0595 Titration Duration 2 06 mm ss Estimated Cell Volume 57 5 mL Titration went to Completion Operator Name Analyst Signature ________________________ ...

Page 191: ...1 TITRATION THEORY TITRATION THEORY Principles HI 903 KARL FISCHER VOLUMETRIC TITRATOR Revision 1 0 ...

Page 192: ...2 TITRATION THEORY ...

Page 193: ...tion 18 4 TITRATIONRESULTS 19 4 1 Accuracy 19 4 2 Repeatability 19 4 3 Sources of Error 19 4 3 1 Sampling Errors 19 4 3 2 Errors with Titrant and Standard 19 4 3 2 1 Preparation Errors 19 4 3 2 2 Dispensing Errors 20 4 3 3 Chemical Reaction Errors 20 4 3 4 End Point Determination Errors 20 5 CALCULATIONS 21 5 1 Equations Used in Karl Fischer Titrations 21 5 1 1 Calculation of water content as mass...

Page 194: ...4 TITRATION THEORY ...

Page 195: ...y or by some other physical measurement Titrations cannot be used to determine the quantity of all analytes The chemical reaction between the titrant and analyte must fulfill four requirements The reaction must be fast and occur within approximately one second after the titrant is added The reaction must go to completion The reaction must have well known stoichiometry reaction ratios A convenient ...

Page 196: ...costs and easy training Suitability to measure major components of a mixture or product Automation can reduce time and labor spent on each analysis Some disadvantages of titrations are Time it takes to prepare standards and titrants Good technique is required to achieve precise results training and practice required Not suitable for determining trace or minor components of a mixture or product Lim...

Page 197: ... point this is due to the change in the electroactivity of the solution Many metal ions can be amperometrically titrated using a precipitation complexation or redox reaction Some metal ions and species that can be determined in this manner include silver barium halides potassium magnesium palladium molybdate sulfate tungstate zinc bismuth cadmium fluoride indium thallium iodine and gold Figure 1 s...

Page 198: ...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 199: ...termination by Karl Fischer titration is based on the reaction described by Bunsen in 1853 in which sulfur dioxide is oxidized by iodine in the presence of water I2 SO2 2 H2O 2 HI H2SO4 In Karl Fischer s 1935 article a new procedure for the titration of water he presented a modified form of the Bunsen reaction adapted for use in determining the water content of non aqueous solutions His titrations...

Page 200: ...er in the titration solution has been reacted The next drop of titrant added to the solution after the equivalence point contains iodine that will remain in the titration solution Thereafter the concentration of iodine in the titration solution increases and the solution develops a yellow and eventually brown color It is difficult even for an experienced analyst to generate reproducible endpoint c...

Page 201: ... excess of iodine has been accounted for during the standardization of the titrant 2 2 2 Acid Base Titrations Acid base titrations are the most common type of titrations Acid base titrations are based upon a reaction between an acid and a base a stoichiometric neutralization or the exchange of protons Virtually all acid base titrations are carried out using a strong acid or a strong base as the ti...

Page 202: ...tometric titrations can be done with Mohr s indicator when all of the chloride has reacted a red silver chromate precipitate is formed or the titration can be easily followed with a silver ISE or chloride ISE for chloride titrations and a reference electrode Figure 4 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...

Page 203: ...ydrogen ion concentration is specifically measured and monitored during the titration process to locate the equivalence point Using an ion selective electrode ISE as the indicator electrode the potentiometric signal in mV is used to directly follow a specific ion s concentration or activity Examples of ISE titrations include titrating fluoride with an aluminum titrant using a fluoride ISE chloride...

Page 204: ...us titrations are usually determined potentiometrically using a pH glass electrode a modified calomel or double junction reference electrode with a low flow rate reference junction Good potentiometric titration curves are obtained in most solvents except those with very low dielectric constants such as benzene chloroform and others when high electrical resistance of the solvent causes unstable pot...

Page 205: ... difference in the total volume of the first reagent added and amount determined from the second titration is the quantity of reagent required to complete the first reaction 2 3 2 Multiple End Point Titrations Under certain conditions some titrations can exhibit more than one equivalence point and be titratable to the individual end points to determine the concentration of each individual componen...

Page 206: ...16 TITRATION THEORY A B Figure 8 Potential glass electrode mV C ...

Page 207: ... known concentration A visual or instrumental indicator for detecting the completion of the reaction A typical manual titration consists of the following steps 1 A volumetric pipette is typically used to add a known volume of sample to the flask 2 An indicator solution or instrument probe is added to the flask 3 A burette is used to measure the addition of titrant to the flask and dispense titrant...

Page 208: ...h very low gear backlash in the burette pump minimal piston seal flexing precision ground inner diameter of the glass syringe a low dead volume valve minimal evaporation permeation and chemically resistant tubing 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 a...

Page 209: ...us or non representative sample Sample changed or was contaminated during collection storage or transfers Poor technique when transferring sample to beaker or flask Errors in the balance calibrate and check balance regularly 4 3 2 Errors with Titrant and Standard 4 3 2 1 Preparation Errors Incorrect preparation due to Poor technique in weighing the salt or when transferring to volumetric glassware...

Page 210: ...first derivative and second derivative The inflection point of a potentiometric 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 D mV vs D V corresponds to the theoretical equivalence point During a titration it is rare to have a data point exactly at the first derivativ...

Page 211: ... Titrant mL Titer Titrant Titer mg mL V sample Volume of Sample mL d sample Density of Sample g mL 5 1 3 Calculation of water content as volume from samples measured by volume C sample Concentration of Sample v v V titrant Volume of Titrant mL Titer Titrant Titer mg mL V sample Volume of Sample mL d water Density of Water at Analysis Temperature g mL 5 1 4 Calculation of water content as mass subt...

Page 212: ...s Samples The water content of gases is normally reported in units of µg L or mg L C sample Concentration of Sample mg L V titrant Volume of Titrant mL Titer Titrant Titer mg mL Flow Rate Sample Flow Rate L min Flow Duration Sample Extraction Time min To calculate the water content in w w the mass of the gas introduced into the titration vessel must be known This can be determined by calculations ...

Page 213: ...ntration g 100g V titrant Volume of titrant 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 m sample Mass of sample g By Volume C sample Sample Concentration g 100mL V titrant Volume of titrant C titrant Titrant Concentration eq L Ratio Equivalence ratio of analyte titrant mol analyte eq titrant F...

Page 214: ...lution matrix The basic titration equation can be used for a blank titration with the single modification that the volume of titrant used in the blank titration should be subtracted from the regular titration titrant volume C Sample 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 ...

Page 215: ...ght of Sample mL 5 2 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 betwe...

Page 216: ...results Back Titration A type of titration where an excess amount of titrant is added to a sample forcing a sluggish reaction to go to completion The excess reagent is then back titrated with a second titrant Base A chemical species that can accept one or more protons hydrogen ions Biamperometric Indication Uses a double platinum pin electrode to measure the current flow through a titration soluti...

Page 217: ...lly used in manual titrations Chemical indicators have been replaced with electrometric indi cators 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 ...

Page 218: ...is determined by monitoring the voltage of the solution using an electrode Precipitation Titration A titration in which the analyte reacts with the titrant to form an insoluble compound The end point is typically detected with an ISE sensitive to either the analyte or titrant Reagent The chemical added in a titration that causes the given reaction to occur Reduction Oxidation Reaction redox A chem...

Page 219: ...olumetric procedure used in analytical chemistry to determine the concentration of an analyte in solution The concentration of the analyte is determined by slowly adding a titrant to the solution As the titrant is added a chemical reaction between the titrant and the analyte occurs Titration Curve A graph containing the physical data obtained for a titration The data plotted is often an independen...

Page 220: ...30 TITRATION THEORY Titr THEORY 903 02 11 ...

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