Hanna Instruments HI 901 Instruction Manual Download

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5-16

METHODS

This is rigorously exact only for symmetric S-shaped titration curves. For non-symmetric curves,

the effect of this theoretical error can be minimized by smaller doses (more measurement

points) around the equivalence point.

1st Derivative:
When first derivative is used to recognize the equivalence point, the point where the first

derivative reaches the maximum value

corresponds to the titration curve inflection point (EQP).

The detection algorithm searches for the maximum value of the first derivative. Also, the first

derivative must be greater than the threshold value at the maximum point (see

Recognition

Options

on page

5-17).

Summary of Contents for HI 901

Page 1: ...I 901 HI 902 AUTOMATIC TITRATOR NaOH Titrant Conc Standardize Electrode General Options Select Method Method Options Burette pH mV ATC Endpoint Volume pH No Result 1300 1300 RPM 15 44 31 Nov 12 2003 N eq L 0 000 NaOH 0 1 M ...

Page 2: ......

Page 3: ...4 GENERALOPTIONS Chapter 5 METHODS Chapter 6 TITRATION MODE Chapter 7 pH mV MODE Chapter 8 AUXILIARYFUNCTIONS Chapter 9 MAINTENANCE PERIPHERALS Appendix 1 TECHNICAL SPECIFICATIONS Appendix 2 BACK TITRATION HI 902 only Appendix 3 MULTIPLE EQUIVALENCE POINTS HI 902 only Appendix 4 ACCESSORIES ...

Page 4: ...uction manual carefully before using the instrument This manual will provide you with the necessary information for the correct use of the instrument 2004 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 5: ...Titration graph can be displayed on line and saved User customized reports can be printed saved on floppy disk or transferred to PC via RS232 interface The sample information and data stamp are included in the report Direct measurements The titrator can also be used for precise mV pH and temperature measurements Report of data logging is available for direct measurements GLP features Up to 5 stand...

Page 6: ...1 2 INTRODUCTION ...

Page 7: ...iew 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 9 2 3 4 5 Attaching the Burette 2 9 2 3 4 6 Electrical Connections 2 1 0 2 3 5 Connection to Earth 2 1 1 2 3 6 Floppy Disk Drive 2 1 1 ...

Page 8: ...2 2 SETUP ...

Page 9: ...5 Burette Blank Support 1 6 Pump and Burette Locking Screws with Plastic Head 2 9 Temperature Sensor 1 10 Shorting Cap 1 11 Power Cable 1 12 RS232 Cable 1 13 Instruction Manual Binder 1 14 Start up Disk FDD with Titrator Installation Kit 1 15 HI 900 PC Application FDD with Installation Kit 1 16 Quality Certificate 1 See Appendix 4 section A 4 3 Titrator components for pictures If any of the items ...

Page 10: ... manual see 9 1 Burette Maintenance section for more details 4 Always check that the titrant bottle and the titration beaker are firmly sitting 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 ...

Page 11: ...2 5 SETUP 2 3 Installation 2 3 1 Titrator Front View 2 3 2 Titrator Rear View NaOH 0 1 M Positioning collar for stirrer adjustment Locking screws input ...

Page 12: ...4 1 Assembling Stirrer Stand and Support Follow these steps to assemble the stirrer Remove the screws 2 from the titrator chassis 1 Attach the stirrer stand 3 to the titrator chassis Make sure to position the stirrer stand close to the wall of the chassis Tighten the stirrer stand 3 using the previously removed screws 2 Screw the stirrer support 4 in the stirrer stand 3 ...

Page 13: ...e stirrer 1 by pressing it onto the stirrer shaft Insert the pH electrode 3 and temperature sensor 4 into the dedicated holes on the stirrer Push them in until they are tightened in a stable position Slide the stirrer on the stirrer support and set the height by tightening the screw located on the positioning collar 5 ...

Page 14: ...ft side bay Connect the cable to the pump as shown in the figure below The pump connector is located in the lower part of the pump near the motor Insert the pump 2 into the dedicated bay Lower the pump until it reaches the lowest position then slide it towards the front of the titrator chassis 1 until it is firmly latched Secure the pump with the loking screw 3 ...

Page 15: ...lowest position then push it toward the front of the titrator chassis 1 until it is firmly latched Secure the burette blank support with the locking screw 5 2 3 4 5 Attaching Burette Make sure that the mark from the valve actuating cap and from the burette body are aligned as shown in the figure below Take care to have a correct coupling between the pump plunger 2 and the syringe piston 1 and also...

Page 16: ...supply 115 230 VAC 50 60 Hz IEC Power line connector 3 Earth connector 5 mm screw 4 Reference electrode Ø 4 mm banana socket 5 Connection for pH or ORP indicating half cell BNC socket or combination electrodes pH mV 6 Temperature sensor RCA socket 7 Stirrer 4 pin mini DIN 8 Connector for expansion device 8 pin DIN socket 9 External PC keyboard 6 pin mini DIN Standard PS2 10 External display Standa...

Page 17: ...he power cord and for added confidence the unit can be connected to Earth using the optional 5 mm screw and the nut connection located on the rear panel of titrator 2 3 6 Floppy Disk Drive Report files new created user methods standard methods can be transferred to and from the titrator using a standard 3 5 floppy disk Connect to Earth optional ...

Page 18: ...2 12 SETUP ...

Page 19: ... 3 4 3 2 1 1 Function Keys 3 4 3 2 1 2 Option Keys 3 4 3 2 1 3 Arrow Keys 3 5 3 2 1 4 Numeric Keys 3 5 3 2 1 5 Enter Key 3 5 3 2 2 Display 3 5 3 2 3 The Main Screen 3 6 3 3 Menu Navigation 3 7 3 3 1 Selecting an Option 3 7 3 3 2 Selecting a Menu Item 3 7 3 3 3 Entering Text 3 7 3 3 4 Saving Modifications 3 8 ...

Page 20: ...3 2 USER INTERFACE ...

Page 21: ...one specified on the titrator are the same 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 fro...

Page 22: ...associated function is immediately performed The and keys are active only in specific screens Displays contextual Help Turns the stirrer ON and OFF Gives access to results menu Reserved Starts or stops a titration or data logging when the titrator is in pH or mV mode 3 2 1 2 Option Keys These keys are assigned to the virtual keys on the display The significance of each option key depends on the me...

Page 23: ...ries 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 graphical display with built in backlight The main screen with short explanations is presented below Temper...

Page 24: ...s the temperature probe is not connected Stirrer information Actual Set stirrer speed is displayed in RPM When stirrer is off the stirrer information is not displayed End point volume Displays the volume delivered to reach the titration end point When no titration has been performed the displayed volume is 0 000 mL Titration result Displays the titration result mV or pH reading Displays the curren...

Page 25: ...oll bar is active on the right side The and keys can be used to scroll through the pages To activate the selected menu item press or 3 3 3 Entering Text To enter text in an alphanumeric input box first erase the previous text by using To enter a letter highlight it using the arrow keys then press Use the same procedure to enter the whole name For editing use the and keys When editing is complete p...

Page 26: ...ress or highlight the Exit Without Saving Method option and then press To save the modifications highlight the Save Method option and then press After the method name is changed it appears in the method name field 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 ...

Page 27: ...te and Time Setting 4 6 4 4 Display Settings 4 7 4 5 Beeper 4 8 4 6 Stirrer 4 8 4 7 Language 4 9 4 8 Daily Standardization Reminder 4 10 4 9 Periodic Standardization Reminder 4 10 4 10 Total Volume Alert 4 10 4 11 Titrant Age Reminder 4 11 4 12 Save Files to Diskette 4 11 4 13 Restore Files from Diskette 4 12 4 14 Serial Link with PC 4 13 4 15 Reset to Default Settings 4 14 4 16 Update Software 4 ...

Page 28: ...4 2 GENERAL OPTIONS ...

Page 29: ...Pump The HI 901 and HI 902 titrators can be equipped with one or two dosing systems pump burette Only one pump can be active at a time This option allows the user to set active either pump 1 or pump 2 Any further operations that involve the pump are referring to the active one Highlight the Active Pump option and then press The Active Pump screen is displayed If there are two pumps connected to th...

Page 30: ...started the active pump will be reset to the one set as default Press and the highlighted pump is set as active immediately in the current session and all following running sessions If only one pump is connected to titrator the Active Pump screen will be as follows 4 2 Temperature The Temperature Menu screen allows selection of temperature source and other options related to temperature ...

Page 31: ...o the ATC icon is displayed When the Manual Temperature option is selected a preset value of the temperature is used for temperature compensation and the Manual icon is displayed on the main screen 4 2 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 op...

Page 32: ...cted The temperature ranges are as displayed in the Temperature Units screen The titrator will automatically convert the measured temperature to the new unit 4 3 Date and Time Setting This screen allows the user to set the date and time By pressing the cursor will cycle to the next field ...

Page 33: ...m black to white is displayed in the center of the display allowing an easy selection of the appropriate display lighting The backlight saver option protects the display during stand by periods when no keys have been pressed for a set amount of time If the display backlight is in Save mode any keystroke will activate the display backlight without performing any action The range for backlight saver...

Page 34: ...beeper to be enabled Beeper On or disabled Beeper Off The beeper will sound after a titration is completed when an invalid key is pressed or when a critical error occurs during titration 4 6 Stirrer This screen allows the stirrer to be enabled or disabled ...

Page 35: ...ion Reminder This screen allows a programmable reminder to appear when it is time to standardize the pH electrode The Standardize Electrode reminder message will appear each day at the programmed time Once standardization has been performed the reminder will disappear until the next day The reminder can be disabled by pressing ...

Page 36: ...new standardization has been performed the reminder will disappear and the timer will reset The reminder can be disabled by pressing 4 10 Total Volume Alert The Total Volume Alert screen allows a programmable reminder to appear when it is time to add supplementary titrant to the glass titrant bottle The current titrant volume data will decrease as the titrant is used The Low Titrant Volume reminde...

Page 37: ... total volume alert was set or since the timer was restarted by pressing The reminder can be disabled by pressing The range is from 0 to 31 days 4 12 Save Files to Diskette This menu allows the user to save files from the titrator to a floppy disk On the titrator the available file types are Standard Method Files HI MTD User Method Files USER MTD Report Files RPT If there is no diskette inserted i...

Page 38: ...rom titrator to floppy disk Returns to the General Options screen The status of the transfer successful unsuccessful and the file name of the currently processed file are displayed during copying or deleting When copying or deleting files is over Press any key message appears and the instrument returns to the list of files 4 13 Restore Files from Diskette This screen allows transfer of files from ...

Page 39: ...ns to the General Options screen All the allowable operations are the same with the ones presented in 4 11 Save Files to Diskette section 4 14 Serial Link with PC In order to use this feature the serial RS232 cable is needed to be connected between the titrator and the PC Make sure that HI 900 PC application is running on the PC In the Serial Communication screen Active Inactive shows the status o...

Page 40: ...urer settings Note Please be careful This will also delete all the user created methods 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 floppy disk ...

Page 41: ...ew Modify Method 5 7 5 5 Method Option 5 8 5 5 1 Naming the User Method 5 8 5 5 2 Titration Type HI 902 only 5 8 5 5 3 Dosing Type 5 9 5 5 3 1 Linear Dosing 5 10 5 5 3 2 Dynamic Dosing 5 11 5 5 4 End Point Mode 5 13 5 5 4 1 Fixed End Point pH or mV 5 13 5 5 4 2 Equivalence End Point pH or mV 5 14 5 5 5 Pre Titration Volume 5 20 5 5 6 Pre Titration Stir Time 5 21 5 5 7 Measurement Mode 5 22 5 5 7 1...

Page 42: ...40 5 5 15 Analyte Size 5 40 5 5 16 Analyte Entry 5 40 5 5 16 1 Fixed Weight or Volume 5 41 5 5 16 2 Manual Weight or Volume 5 41 5 5 17 Titrant 1 Entry HI 902 only 5 41 5 5 17 1 Calculated by Formula 5 41 5 5 17 2 Fixed by User 5 41 5 5 18 Maximum Titrant Volume 5 42 5 5 19 Stirring Speed 5 42 5 5 20 Potential Range 5 43 5 5 21 Volume Flow Rate 5 43 5 5 22 Signal Averaging 5 44 5 6 Printing 5 44 ...

Page 43: ...to a method The titrator is supplied with a pack of standard methods Using a floppy disk or connect the titrator to a PC using the HI 900 PC application the methods standard and user methods can be upgraded stored or deleted 5 1 Selecting Methods To select a method press from the main screen A list of available methods will be displayed In the Titration Methods screen you can view the list of all ...

Page 44: ...tandard methods To upgrade the titrator from Floppy Disk or PC with new standard methods folow the steps below Floppy Disk Insert the methods installation diskette into the floppy disk unit Press from the main screen Using and keys highlight the Restore Files from Diskette option and choose Using and keys navigate through file types menu to find standard method files The list with available standa...

Page 45: ...d methods Press to return to General Options screen Also you can remove standard methods from the titrator using the HI 900 PC application see 4 14 Serial Link with PC section 5 2 3 Restore the Standard Methods to the Manufacturer Settings You can restore the standard methods to the manufacturer setting by highlighting a standard method and pressing Warning Be careful by pressing you will also del...

Page 46: ...erated Press to activate the new created user method Note Only a limited number of user methods can be generated If the limit of standard and user methods 100 methods is reached a warning message will be displayed 5 3 2 Deleting User Methods To remove a user method press from the main screen Highlight the user method that you want to delete and press A screen will appear in order to confirm the de...

Page 47: ...screen A list of all the parameters for the selected method will be displayed Using the and keys highlight the option that you want to modify and choose Save method From the View Modify Method screen press You can choose to save the modifications of the method parameters or to discard them ...

Page 48: ...s Use the arrow keys to navigate through the character table Press to add the highlighted character to the method name 5 5 2 Titration Type HI 902 only In order to make an analysis you have to choose the type of titration Standard Titration A titration with a pH or mV equivalence point detection A titration with fixed pH or mV end point ...

Page 49: ...ly the concentration of the sample will be determined Also if the Back Titration option is chosen the following settings must be selected Titrant 1 pump select the pump used in phase 1 of the titration Pump 1 Titrant 2 pump select the pump used in phase 2 of the titration Pump 2 Break at titrant changing select YES to stop titration temporarily between the first and the second phase of the back ti...

Page 50: ...aqueous titrations or certain specific analysis Note For steep and normal titration curves smaller volume increments are recommended to obtain many measured points around the equivalence point For flat titration curves larger volume increments are recommended for equivalence point detection To set the dosing volume select Linear Dosing option and type the optimum dose Linear Dosing ...

Page 51: ... titrant dose by trying to maintain a certain potential change delta E with each addition If the potential jump after the titrant dose is lower than the set delta E the next dose volume is progressively increased until max Vol is attained If the potential jump is still lower the titration will continue with the max Vol doses If the potential jump after the titrant dose is higher than the set delta...

Page 52: ... delta E Sets the fixed potential jump that has to be achieved after each titrant dose The allowed range is between 0 1 and 99 9 mV Recommendations for dosing parameters For titrations with stepper 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 titrations with flat titration curves th...

Page 53: ...he titration is normally terminated when the preset pH value has been exceeded The reported end point volume is interpolated between the dispensed volume when pH is under the preset pH value and the dispensed volume when pH exceeded the preset pH value The range is from 2 000 to 20 000 pH ...

Page 54: ...is expressed in mV The range is from 2000 0 to 2000 0 mV 5 5 4 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 according to the chemical combination ratio ...

Page 55: ...more doses to be dispensed in the analyte after the equivalence point is reached The reported end point volume is a calculated value based on a number of points around the equivalence point The potentiometric S shaped titration curve is the response in potential mV or pH between the indication of the electrode versus cumulated addition of titrant The graph takes the shape of the S character and ca...

Page 56: ...uivalence point 1st Derivative When first derivative is used to recognize the equivalence point the point where the first derivative reaches the maximum value corresponds to the titration curve inflection point EQP The detection algorithm searches for the maximum value of the first derivative Also the first derivative must be greater than the threshold value at the maximum point see Recognition Op...

Page 57: ...erivative corresponding to the checked point must be greater than the threshold value see Recognition Options on page 5 17 Recognition Options The Recognition Options screen represents a set of parameters used to avoid false detection of the equivalence point This could appear mainly due to the chemical system involved titrant sample chemical species and concentrations and or to the electrode resp...

Page 58: ...w which the detection algorithm does not search for the equivalence point Range is between 1 and 9999 mV mL The recommended value for the threshold is around 40 of the estimated maximum absolute value of the first derivative Depending on the titration curve profile the following guiding ranges might be used TITRATION CURVE PROFILE THRESHOLD mV mL FLAT 1 to 450 NORMAL 450 to 1800 STEEP 1800 to 9999...

Page 59: ...it of the range attained during the titration This range can be from 2 000 pH to 20 000 pH for pH equivalence point This range can be from 2000 0 mV to 2000 0 mV for mV equivalence point Limit 2 The second limit of the range attained during titration This range can be from 2 000 pH to 20 000 pH for pH equivalence point This range can be from 2000 0 mV to 2000 0 mV for mV equivalence point The Limi...

Page 60: ...ettings such as Signal Stability Stirring Speed etc Too small titrant doses Note Even if false equivalence point detection has been highly diminished a shift of the end point volume might sometimes occur due to filtering The shift is often at the level of 1 or 2 doses from the real equivalence point volume For fast titrations and small doses this is a useful option 5 5 5 Pre Titration Volume Durin...

Page 61: ...used 0 000 mL should be entered Note A pre titration volume is highly recommended whenever possible When fewer linear doses are used the overall titration duration considerably shortens 5 5 6 Pre Titration Stir Time When this option is enabled the sample is mixed for a period of time before the titration begins This allows the sample to become homogeneous The range is from 0 to 180 seconds If 0 se...

Page 62: ...tion Addition of the next dose is performed immediately after the potential is measured 5 5 7 1 Signal Stability When Signal Stability option is selected the titrator acquires the potential from solution only when the stability condition is reached The response of the electrode for each added dose and the principles of the stability window are plotted below and described on the following page ...

Page 63: ...d the potential is acquired and a new dose is added delta E is the height of the signal stability window The range is from 0 1 to 99 9 mV delta t is the width of the signal stability window The range is from 0 5 to 10 0 seconds t min wait is the minimum elapsed time before 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 w...

Page 64: ... the acquiring of the potential mV value from the solution is made at a fixed time interval no signal stability check The time period between two acquisitions must be set according with the used reaction and the time response of the electrode The range is from 2 to 180 seconds ...

Page 65: ...rs The electrode type will appear in the titration report 5 5 9 Blank Option This feature allows the user to select the procedure for the blank calculations where V is the volume of titrant dispensed during the titration and Blank is the volume of titrant consumed by the blank sample ...

Page 66: ...ode is set the Imposed Current option will become available Using the imposed current feature in end point redox titrations has a great advantage on the speed of the redox reactions The speed is increased significantly when the double Pt electrode used for the titration is polarized with a small imposed current we obtain a stepper jump perfect adapted for end point titrations In order to use this ...

Page 67: ...omputed starting from the end point volume titrant volume at the equivalence point using a formula set by the user 5 5 11 1 Standard Titrations Edit Variable Values This option allows the user to change the values of the variables used in a previously selected calculation For each formula selected variables can be changed No Formula mL only If this option is selected only delivered milliliters mL ...

Page 68: ...ide the results based on the titrant and sample units selected Titrant Units M mol L moles liter N eq L equivalences liter g L grams liter mg L milligrams liter Final Result Units ppt g Kg parts per thousand grams kilogram ppm mg Kg parts per million milligrams kilogram ppb µg Kg parts per billion micrograms kilogram g 100 g percentage in weight grams 100 grams mg g milligrams gram mg Kg milligram...

Page 69: ...n analyte is determined in a liquid 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 perform the calculation based on the titrant and the sample units selected Titrant Units M mol L moles liter N eq L equivalences liter g L grams liter mg L milligrams liter Final Sample ...

Page 70: ...If the titrant unit is selected as N eq L and the final sample unit as g L grams liter the formula used to generate the result is displayed below Some variables can be set according to the amount of sample and titrant used Standardize Titrant by Weight This calculation should be used when the titrant is standardized concentration determination using a solid standard Determination of the titrant co...

Page 71: ... solid or liquid sample The variables can be set to reach any final result from the list below ppt g Kg parts per thousand grams kilogram ppt g L parts per thousand grams liter ppm parts per million milligrams kilogram ppm mg L parts per million milligrams liter ppb parts per billion micrograms kilogram ppb µg L parts per billion micrograms liter g 100 g percentage in weight grams 100 grams M mol ...

Page 72: ...r titrant standardization or for sample analysis C V F1 F2 F3 S Where C the concentration of the titrant F1 general factor F2 general factor F3 general factor S sample size in grams or milliliters V the volume delivered in liters to reach the preset or equivalence end point determined by the titrator ...

Page 73: ...titrant or standard and titrant In the particular case that the combination ratio is expressed in moles this factor is called the stoichiometric factor This factor can be one of the following mol mol moles of sample moles of titrant mol eq moles of sample equivalence of titrant eq mol equivalences of sample moles of titrant mol mol moles of titrant moles of standard eq mol equivalences of titrant ...

Page 74: ...5 34 METHODS 5 5 11 2 Back Titrations HI 902 only Sample Calculations by Weight When choosing this formula select the titrant 1 unit the titrant 2 unit and then the final result unit ...

Page 75: ... it with an excess factor in order to raise or to lower the amount of titrant 1 dispensed Some variables can be set according to the amount of sample and titrant 1 used When the parameters from the formula are set press to proceed with the next formula used in the back titration algorithm If you do not want to use the Calc Direct Titr Volume formula then from the View Modify Method screen highligh...

Page 76: ...volume of titrant 1 is calculated the following formula is used to calculate the exact volume of titrant 1 that was consumed by the sample V1 V1tot V1excess When all the parameters are set press to proceed with the Calculating Sample Concentration formula Sample Calculations by Volume When choosing formula follow these steps First select the titrant 1 unit ...

Page 77: ...ill provide the calculation based on the titrants and sample units selected After you have selected the titrant 1 titrant 2 and the final result units the titrator will display a screen with a formula used to calculate the amount of titrant 1 used in the first stage of back titration ...

Page 78: ...th this approximation the titrator will calculate the volume of titrant 1 needed to consume the sample and multiply it by an excess factor in order to raise or to lower the amount of titrant 1 dispensed When the parameters from the formula are set press to proceed to the next formula used in the back titration algorithm This formula is used to calculate the remaining volume of titrant 1 after the ...

Page 79: ...liquid sample 5 5 12 Dilution Option This option enables the dilution calculations to be made when the initial sample is diluted the titration is made with an aliquot of the diluted sample The calculations are made for the sample weight volume in order to express the results for the initial sample Final Dilution Volume The volume of the sample after the dilution process Aliquot Volume The volume o...

Page 80: ...tration report 5 5 14 Titrant Concentration Enter the concentration of the titrant to be used When determining the titrant concentration only the unit is displayed and the titrant concentration can not be set 5 5 15 Analyte Size Enter the size of the sample for sample concentration determinations or standard for titrant concentration determination 5 5 16 Analyte Entry With this option select the e...

Page 81: ... beginning of each titration 5 5 17 Titrant 1 Entry HI 902 only Select the mode for evaluating the necessary quantity of titrant 1 used in the back titration process phase 1 5 5 17 1 Calculated by Formula The volume of titrant 1 to be dispensed in the phase 1 of back titration will be calculated by formula see Calc Direct Titr Volume screen on page 5 35 5 5 17 2 Fixed by User Fixed volume of titra...

Page 82: ...fter the maximum titrant volume has been dispensed The error message Limits Exceeded will appear on the display Range is from 0 100 to 100 000 mL 5 5 19 Stirring Speed The stirring speed can be set between 100 and 2500 RPM with 100 RPM resolution The preset value of stirrer speed from the current method is used during the entire process as long as the method is set as active Also the speed can be ...

Page 83: ...n end point due to potential over range The ranges must be set within 2000 0 to 2000 0 mV 5 5 21 Volume Flow Rate The flow rate for the dosing system can be set by the user in an interval of 0 1 to twice the total burette volume as follows 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 0 1 to 100 mL min for a 50 mL burette Note The tit...

Page 84: ... 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 6 Printing To print method parameters press from the main screen Press and wait a few seconds until the printer completes the job If no printer is connected to the dedicated socket or if the printer is offline an error message will appear on ...

Page 85: ...6 1 TITRATION MODE Chapter 6 Contents 6 TITRATION MODE 6 3 6 1 Titration Start 6 3 6 1 1 In Progress Titration 6 3 6 1 2 Suspend Titration 6 3 6 1 3 On line Graph 6 3 6 2 Titration Stop 6 5 ...

Page 86: ...6 2 TITRATION MODE ...

Page 87: ... stirring time option is enabled the sample will be stirred until the prescribed time elapses see 5 5 6 Pre Titration Stir Time If the pre titration volume option is enabled the prescribed volume will be dis pensed see 5 5 5 Pre Titration Volume According to the Measurement Mode and the Dosing Type option the titrator will start to deliver doses until the titration end point are detected or a titr...

Page 88: ...nd Point pH the pH curve and the selected derivative vs volume is displayed see Figure 1 Equivalence End Point mV the mV curve and the selected derivative vs volume is displayed see Figure 2 Fixed End Point pH only the pH vs volume curve is displayed see Figure 3 Fixed End Point mV only the mV vs volume curve is displayed see Figure 4 Figure 1 Figure 2 Figure 3 Figure 4 allows you to view on the o...

Page 89: ...lly Terminated The current titration was manually terminated before end point detection was achieved Limits Exceeded The preset maximum titrant volume was delivered without reaching the end point The titration is stopped with an error message Critical Error A critical error occurred and the titration was stopped These errors are normally related to the dosing system The titration is stopped with a...

Page 90: ...6 6 TITRATION MODE ...

Page 91: ...3 Clear Standardization 7 5 7 1 2 4 Edit Buffer Set 7 5 7 1 2 5 Graph Standardization Data 7 6 7 1 2 6 pH Standardization Data 7 6 7 1 2 7 Resolution 7 6 7 2 mV Mode 7 6 7 2 1 Display 7 6 7 2 2 mV Menu 7 7 7 2 2 1 Auto Zero Relative mV 7 7 7 2 2 2 Enter a Manual Relative mV 7 7 7 2 3 1 Clear Relative mV Offset 7 8 7 3 Logging 7 8 7 3 1 Automatic Logging 7 9 7 3 2 Manual Logging 7 9 ...

Page 92: ...7 2 pH mV MODE ...

Page 93: ...en 7 1 pH Mode 7 1 1 Display The pH screen shown below will help you understand the following explanations pH Mode Option keys Brings you to the General Options screen for more details see Chapter 4 General Options Stores the current pH reading see section 7 3 2 Manual logging Displays the setup options for pH see section 7 1 2 pH Menu Switches to the mV screen Return to the main screen Temperatur...

Page 94: ... automatically recognized and temperature compensated from the created buffer list see section 7 1 2 4 Edit Buffer Set The titrator accepts electrode s slope between 80 to 105 7 1 2 2 Add a Buffer Manual Entry The user can add a custom buffer to the calibration list The titrator will prompt for the custom buffer value The buffer value entered should be correlated with the expected temperature valu...

Page 95: ...d from the set described below Available buffers include Hanna 4 01 6 86 7 01 9 18 10 01 CRC 1 68 3 56 4 01 6 87 7 41 9 18 12 46 DIN 1 09 3 06 4 65 6 79 9 23 12 75 NIST 4 01 6 86 7 42 To select a buffer from the list highlight the desired buffer and press to add it to the buffer set The selected buffers are marked with an asterisk Note Although any combination of buffers may be selected their valu...

Page 96: ...creen shown below will help you understand the following discussion mV Mode Option Keys Brings you to the General Options screen for more details see Chapter 4 General Options Stores the current mV reading see section 7 3 2 Manual logging Displays the setup options for mV see section 7 2 2 mV Menu Switches to the pH screen Return to the main screen mV Value Time and Date Temperature Compensation S...

Page 97: ...h a shorting cap before performing this action Note The auto zero will affect the mV reading and therefore the pH value new displayed relative mV reading will be used to calculate the new pH value 7 2 2 2 Enter a Manual Relative mV Allows to enter the mV offset The range is from 2000 0 to 2000 0 mV The set value is subtracted from the actual readings from electrode In this case the actual readings...

Page 98: ...on please customize a unique report for the saved pH and mV measurements as follows From the pH or mV screen press to display the Data Parameters screen Highlight the Setup pH mV Report option and press to display the Setup pH mV Report screen Use the and keys to highlight the data field that you want to show hide in the pH mV report and then press to activate deactivate it Each field marked by is...

Page 99: ...nsecutive record The time between records can be set in the following range Hours 0 to 8 Minutes 0 to 59 Seconds 0 to 59 Press and then to save the setting and return to the pH or mV screen Press to start auto logging The logging interval and name of logging file will be also displayed on the pH or mV screen To stop the automatic logging press again 7 3 2 Manual Logging To manually log pH or mV re...

Page 100: ...7 10 pH mV MODE ...

Page 101: ... Rinse Tip 8 4 8 1 3 Manual Dispense 8 4 8 1 4 Purge Burette 8 5 8 2 Stirrer 8 5 8 3 Results 8 6 8 3 1 Review Last Titration Report 8 6 8 3 2 Review Available Reports 8 6 8 3 3 GLP Data 8 7 8 3 4 Instrumentation Data 8 8 8 3 5 Logging Interval pH mV 8 9 8 3 6 Setup pH mV Report 8 9 8 3 7 Setup Titration Report 8 9 ...

Page 102: ...8 2 AUXILIARY FUNCTIONS ...

Page 103: ...rime Burette option is used to mechanically fill the burette before starting a set of analysis Two rinses cycles of burette are shown in the figure below The dispensing tube is connected on the right side and the aspiration tube on the left side Note Before starting this operation the aspiration tube must be inserted in the titrant bottle 8 AUXILIARY FUNCTIONS ...

Page 104: ...e completely removed 8 1 2 Rinse Tip A 2 mL dose of titrant will be dispensed from the burette when this operation is started This operation will eliminate the air from the dispensing tip 8 1 3 Manual Dispense Using the Manual Dispense option a defined titrant volume can be dosed Select the Manual Dispense option and press The Manual Volume Dispense screen will become active and the display will p...

Page 105: ...ws titrant evacuation before cleaning and or storing the burette The burette is flushed twice Note Before starting this operation remove the aspiration tube from the titrant bottle The figures below show the steps in a purge burette operation 8 2 Stirrer The stirrer can be started and stopped by pressing The stirring speed is set within the active methods see section 5 5 17 Stirring Speed During t...

Page 106: ...e information that can be reviewed in the report is based on the selections made in the Setup Titration Report screen The following option keys are available Allows review of the last performed titration graph The pH or mV versus titrant volume curve can also be displayed Also if the Equivalence End Point option was selected the pH or mV curve and selected derivative curve 1st derivative 2nd deriv...

Page 107: ...up Titration Report and Setup pH mV Report screens during report configuration The keys are the same as in the previous section 8 3 1 Review Last Titration Report Allows you to delete the selected report 8 3 3 GLP Data Enter up to 20 alphanumeric characters for each option from GLP Data screen Sample Name Allows the sample name to be recorded in each report The sample name will increase by one wit...

Page 108: ...2 Serial Number Indicates the serial number of the titrator analog board 2 Pump 1 and or 2 Serial Number Indicates the serial number of each connected pump Titrator Software Version Indicates the current software version installed on the titrator Base Board Software Version Indicates the current software version present on the base board of the titrator Pump 1 and or 2 Software Version Indicates t...

Page 109: ...uto logging while in pH or mV mode see 7 3 Logging section 8 3 6 Setup pH mV Report Customize a unique report to record the pH and mV measurements 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 ...

Page 110: ...8 10 AUXILIARY FUNCTIONS ...

Page 111: ...rette 9 3 9 1 3 Disassembling Burette 9 4 9 1 4 Assembling Burette 9 4 9 1 5 Cleaning 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 ...

Page 112: ...9 2 MAINTENANCE PERIPHERALS ...

Page 113: ...the accessories mounted see 2 1 Unpacking section for burette assembly details Note The dispensing tube has one flat shaped end and the other one is equipped with a dispensing tip See 2 1 Unpacking section for the accessories list 9 1 2 Changing Burette Remove the burette from the pump assembly by sliding it back and then slide the new burette into place see the picture below ...

Page 114: ...nd a protection tube The aspiration tube will be mounted in the left side and the dispensing tube will be mounted in the right side of the burette see diagram on the next page To attach the dispensing tube and the aspiration tube follow these steps Slide the mounting tool 3 over the dispensing tube Insert the flat shaped end of the dispensing tube into the valve outlet Screw in the fitting 2 with ...

Page 115: ...nt solvent to clean the tube Execute prime burette operation to fill the burette use 2 rinses see 8 1 1 Prime Burette section During second refilling of the burette remove the aspiration tube out of the solvent beaker 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 for the desired purpose continue with the...

Page 116: ...syringe and piston to remove aggressive chemicals Do not touch the Teflon part of the piston and internal walls of the 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 ...

Page 117: ... 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 and a little air zone just above the liquid level at the first filling movement The next upward movement will evacuate the entire air This way n...

Page 118: ... Replace the fuses for recommended fuses replacement please see the label located above the main 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 ...

Page 119: ...play 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 9 3 2 Connecting an External PC Keyboard This connection allows you to use an external PC Keyboard in addition to titrator s keypad Connect an external PC Keyboard having a 6 pin Mini DIN connector ...

Page 120: ...3 Function Key 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 Alphanum...

Page 121: ...r and the external printer must be both turned OFF from the main switch before making the connection 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 standard serial cable with a standard DB9 pin connector HI 900 PC application needs to be installed on the PC ...

Page 122: ...cable to the serial communication port on the PC Turn on the titrator and then the computer Select the Serial Communication screen on the titrator following the path General Options Serial Link with PC Serial Communication Launch the HI 900 PC application and then select the appropriate serial port on the PC The HI 900 PC application allows the transfer of a variety of information between titrator...

Page 123: ...A1 1 APPENDIX 1 Appendix 1 Contents A1 TECHNICAL SPECIFICATIONS A1 3 ...

Page 124: ...A1 2 APPENDIX 1 ...

Page 125: ...ods 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 Programmable Stirring Speed 100 2500 RPM automatically held with a 100 RPM accepted tolerance Flow Rate user selectable see 5 5 21 Volume Flow Rate section for ranges Direct mV pH Measureme...

Page 126: ...s Files Copied to and Restored from Floppy Disk Standard Methods User Methods Titration and pH mV Logging Reports Graphic Bitmap Files can be transferred to and from floppy disk using the 3 5 Floppy Disk unit of the titrator Peripheral Units Attachment Possibilities External VGA Display External PC Keyboard Printer RS232 interface GLP Conformity Good Laboratory Practice and Instrumentation Data st...

Page 127: ...ON HI 902 only A2 3 A2 1 Applicability Domain A2 3 A2 2 Method Principles A2 3 A2 3 Back Titration Example 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 ...

Page 128: ...A2 2 APPENDIX 2 ...

Page 129: ...m the sample With this reagent quantity will be calculated the sample concentration The back titration can be an acid base complexometric redox etc A2 3 Back Titration Example An example of back titration might be the determination of an antacid neutralizing capacity A2 3 1 Introduction An excess of stomach acid primarily HCl causes heartburn and acid indigestion Commercial antacids consist of a n...

Page 130: ...Der Recognition Option Threshold 500 mV mL Range NO Filtered Derivatives NO Pre Titration Volume 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 mo...

Page 131: ...e bottom of the beaker Adjust the level of the sample solution 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 If the method is selected the main screen displays Antacid Power at method name press The titrator will prompt for the sample weight Enter the exact weight value with 4 ...

Page 132: ...ere with the titration Cool the solution to the room temperature and put the beaker under the stirrer asembly Lower the stirrer assembly until it rest on its positioning collar Adjust the height of the stirrer by using the positioning screw of the positioning collar to have the propeller as close as possible to the bottom of the beaker Press to proceed to the second phase of the analysis This phas...

Page 133: ...A3 1 APPENDIX 3 Appendix 3 Contents A3 MULTIPLE EQUIVALENCE POINTS HI 902 only A3 3 A3 1 Applicability Domain A3 3 A3 2 Perform a Multi Equivalence Point Titration A3 3 A3 3 Titration Example A3 4 ...

Page 134: ...A3 2 APPENDIX 3 ...

Page 135: ...t s titrable ionization stages e g H3PO4 two equivalence points in aquogenos medium A3 2 Perform a Multi Equivalence Point Titration With the information provided above set up the method parameters as follows Set the end point mode as equivalence end point mV or pH Set the number of equivalence points up to 5 points to be found Select the end point determination like in standard titration Set the ...

Page 136: ...H4 CL with 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 all the equivalence points detected ...

Page 137: ...g for the first equivalence point marked with a cross the next volumes marked with a cross are calculated as the difference betwen the total volume dispensed until the current equivalence point is reached and the sum of the already detected equivalence points The concentration is calculated with the formula selected in the Calculations option from the View Modify Method screen ...

Page 138: ...A3 6 APPENDIX 3 ...

Page 139: ...torage Solutions A 4 4 A4 1 6 Electrode Storage Solutions in FDA Approved Bottle A 4 4 A4 1 7 Refilling Electrolyte Solutions A 4 4 A4 1 8 Refilling Electrolyte Solutions in FDA Approved Bottle A 4 4 A4 1 9 ORP Pretreatment Solutions A 4 4 A4 1 10 Titration Reagents A 4 4 A4 2 Sensors A4 5 A4 2 1 pH Electrodes A 4 5 A4 2 2 ORP Electrodes A 4 6 A4 2 3 Half cell Electrodes A 4 6 A4 2 4 Extension Cab...

Page 140: ...A4 2 APPENDIX 4 ...

Page 141: ...10M pH 10 01 Buffer Solution 230 mL HI 7010L pH 10 01 Buffer Solution 500 mL HI 7001M pH 1 68 Buffer Solution 230 mL HI 7001L pH 1 68 Buffer Solution 500 mL A4 1 2 pH Calibration Solutions in FDA Approved Bottle HI 8004L 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 Sol...

Page 142: ...te 30 mL HI 7082 3 5M KCl Electrolyte 30 mL for double junction electrodes A4 1 8 Refilling Electrolyte Solutions in FDA Approved Bottle HI 8071 3 5M KCl AgCl Electrolyte 30 mL for single junction electrodes HI 8072 1M KNO3 Electrolyte 30 mL HI 8082 3 5M KCl Electrolyte 30 mL for double junction electrodes A4 1 9 ORP Pretreatment Solutions HI 7091M Reducing Pretreatment Solution 230 mL HI 7091L Re...

Page 143: ...unction refillable combination pH electrode Use laboratory HI 1331B HI 1311S Glass body semimicro single junction refillable combination pH electrode Use flasks HI 1230B HI 1210S Plastic body Ultem double junction gel filled combination pH electrode Use general purpose HI 2031B HI 2020S Glass body semimicro conic refillable combination pH electrode Use semisolid products HI 1332B HI 1312S Plastic ...

Page 144: ...dy refillable combination platinum ORP electrode Use titration HI 3230B HI 3210S Plastic body Ultem gel filled combination platinum ORP electrode Use general purpose HI 4430B HI 4410S Plastic body Ultem gel filled combination gold ORP electrode Use general purpose A4 2 3 Half cell Electrodes HI 2110B Glass body single half cell pH electrode Use general purpose HI 5311 Glass body Ag AgCl reference ...

Page 145: ...lectrodes only Screw to BNC Connector HI 7855 1 Extension cable 1m 3 3 long A4 2 5 Temperature Sensor HI 7662 T Temperature probe with 1 m 3 3 paneled cable Ultem is registered Trademark of General Electric Co Kynar is registered Trademark of Pennwalt Corp ...

Page 146: ...pensing tip fitting protec tion tube and tube guide Tube locks Tool for valve fitting and burette cap removal Light spectrum protection screen Overhead Stirrer Propeller Stirrer support with positioning collar and positioning screw Stirrer stand Burette blank support Pump and burette locking screw with plastic head Temperature Probe Power Cable RS232 Cable ...

Page 147: ...APPENDIX 4 Shorting cap Instruction Manual Binder Start up Disk FDD with Titrator Installation Kit H I 9 0 1 9 0 2 H I 9 0 1 9 0 2 HI 900 Series Titration Systems Ww w h ann ainst c om Ww w h ann ainst c om ...

Page 148: ...A4 10 APPENDIX 4 MAN901 902 09 04 R0 ...

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