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5-15

TITRA

TION METHODS

5.5.7. RECOGNITION OPTIONS (EQUIVALENCE END POINT ONLY)

The 

Recognition Options

 screen is a set of parameters used to avoid false detection of the equivalence point due to the chemical 

system (titrant/sample species and concentrations) and/or electrode response.

5.5.7.1.    THRESHOLD

Option: 1 to 9999 mV/mL

This parameter must be set by the user according to the analysis.
The threshold represents the absolute value of the first derivative, expressed in mV/mL, below which the detection algorithm does not 
search for the equivalence point.

The recommended value is 40% of the absolute value of the first derivative.

Summary of Contents for HI931

Page 1: ...MANUALS AUTOMATIC POTENTIOMETRIC TITRATOR HI931 ...

Page 2: ......

Page 3: ...ive description of the operating principles user interface general options methods titration direct reading mode pH mV and ISE mode maintenance etc APPLICATIONS BROCHURE This brochure contains complete instructions for commonly used analyses Additional methods and method packs are available contact your local Hanna office for more details TITRATION THEORY This guide outlines the principles of oper...

Page 4: ......

Page 5: ...QUICK START GUIDE AUTOMATIC POTENTIOMETRIC TITRATOR HI931 ...

Page 6: ...e purpose of this guide is to present a quick overview of setting up and using the instrument For detailed information illustrating the extensive capabilities of your titrator please refer to the Instruction Manual Dear Customer 2018 Hanna Instruments All rights are reserved Reproduction in whole or in part is prohibited without the written consent of the copyright owner Hanna Instruments Inc Woon...

Page 7: ... GUIDE INTRODUCTION SAFETY MEASURES TITRATOR CONNECTIONS USER INTERFACE HOW TO SELECT YOUR LANGUAGE HOW TO USE THE CONTEXTUAL HELP METHODS HOW TO CALIBRATE A pH ELECTRODE HOW TO PERFORM A TITRATION 4 5 7 7 8 4 6 7 7 ...

Page 8: ...uction Manual provides a complete description of the operating principles user interface general options methods titration pH mV and ISE mode maintenance etc The Titration Theory outlines the basic concepts of titration The contextual Help screens contain detailed explanations of every screen SAFETY MEASURES The following safety measures must be followed 1 Never connect or disconnect the pump asse...

Page 9: ...5 QUICK START GUIDE TITRATOR CONNECTIONS FRONT VIEW REAR VIEW ...

Page 10: ...categories as follows Display The user interface contains several screens In each screen many information fields are present at the same time The information is displayed in an easy to read manner Virtual option keys describe the function performed when the corresponding option key is pressed ...

Page 11: ...wine dairy etc User Defined Methods User defined methods allow the user to create and save their own methods Each new method is based on an existing method which is altered to suit a specific application HOW TO CALIBRATE A pH ELECTRODE To enter pH calibration mode press then then PREPARATION Pour small quantities pH 4 01 pH 7 01 and pH 10 01 buffer solutions into clean beakers If possible use plas...

Page 12: ...ation tube in the titrant bottle and the dispensing tube in a waste beaker From the main screen press Highlight the Prime Burette option and then press Enter the number of burette rinses At least 3 rinses are recommended Press to start The message Executing will be displayed Note Make sure you have continuous liquid flow inside the burette For accurate results the aspiration tube the dispensing tu...

Page 13: ...ker Slide the stirrer assembly up Place the beaker under the stirrer assembly Lower the stirrer assembly until the electrodes are submersed and the stirrer is close to the bottom of the beaker Adjust the level of the sample solution with distilled deionized water so that the pH electrode bulb is completely immersed in the sample solution and the reference junction of the electrode is 5 6 mm below ...

Page 14: ...he same screen window Press to change the y axis scale to either the pH values or the 1st derivative values Titration Termination The titration is normally terminated when the first equivalence endpoint is detected according to the selected algorithm To ensure the correct detection and interpolation of the equivalence endpoint the titrator will dispense a few additional doses after the endpoint wa...

Page 15: ...reen will be displayed Use the and keys to display information related to the last titration performed See Titration Report on next page Printing the titration report Connect a DOS Windows compatible parallel printer directly to the DB 25 pin connector located on the back of the titrator Note When connecting the printer please turn off the titrator and the printer Printing out the report From the ...

Page 16: ...l Number DP180525004 Stirrer 1 Serial Number OS180524001 Analog 1 Calibration Date May 25 2018 Method Parameters Name Neutralization w NaOH Method Revision 3 0 Analysis Type Standard Titration Stirrer Configuration Stirrer Stirrer 1 Stirring Speed 1400 RPM Use the and keys to select the report files Press to transfer all available reports to the USB storage device or highlight the name of the repo...

Page 17: ...V Volume Flow Rate 25 mL 50 0 mL min Signal Averaging 1 Reading Significant Figures XXXXX N eq L meq L V eq 1000meq L eq mL L 1000mL V volume dispensed in liters 0 100 eq L titrant conc 10 000 mL sample volume Nr Volume mL mV pH Graphic Temp C Time 0 0 000 274 4 2 219 0 0 24 9 A 00 00 00 1 0 050 274 4 2 220 1 0 25 0 A 00 00 07 2 0 100 274 4 2 220 0 0 25 0 A 00 00 10 3 0 200 274 3 2 222 0 8 25 0 A ...

Page 18: ...5 1 A 00 02 28 20 6 278 174 5 9 903 335 8 25 1 A 00 02 35 21 6 339 187 8 10 130 215 9 25 1 A 00 02 42 Titration Results Method Name Neutralization w NaOH Time Date 15 01 Jun 13 2018 Analyte Size 10 0000 mL End Point Volume 6 144 mL pH Equivalence Point 8 063 Result 61 444 meq L Initial Final pH 2 219 to 10 130 Titration Duration 2 42 mm ss Titration went to Completion Analyst Signature ___________...

Page 19: ...INSTRUCTION MANUAL AUTOMATIC POTENTIOMETRIC TITRATOR HI931 ...

Page 20: ......

Page 21: ...cise idea of its versatility If you need additional technical information do not hesitate to e mail us at tech hannainst com or view our worldwide contact list for a Hanna Instruments representative near you at www hannainst com Dear Customer 2018 Hanna Instruments All rights are reserved Reproduction in whole or in part is prohibited without the written consent of the copyright owner Hanna Instru...

Page 22: ...NERAL OPTIONS CHAPTER 5 TITRATION METHODS CHAPTER 6 TITRATION MODE CHAPTER 7 pH MODE CHAPTER 8 mV MODE CHAPTER 9 ISE MODE CHAPTER 10 AUXILIARY FUNCTIONS CHAPTER 11 MAINTENANCE PERIPHERALS APPENDIX 1 TECHNICAL SPECIFICATIONS APPENDIX 2 ACCESSORIES CERTIFICATION RECOMMENDATIONS FOR USERS WARRANTY ...

Page 23: ...trode holder supports up to 3 electrodes 4 dispensing tubes 1 temperature sensor and removable stirrer Electrode holder positions electrodes in the center of beaker allowing for smaller sample sizes Integrated Peristaltic Pump available for reagent addition Support for 100 titration methods User customizable reports Integrated research grade pH mV ISE meter Clearly displayed warning and error mess...

Page 24: ...1 2 ...

Page 25: ... 3 4 TITRATOR RIGHT SIDE VIEW 2 3 5 TITRATOR ASSEMBLY 2 3 5 1 ASSEMBLING STIRRER AND ELECTRODES HOLDER 2 3 5 2 ATTACHING STIRRER AND ELECTRODES 2 3 5 3 CONNECTING THE PUMP 2 3 5 4 ATTACHING BURETTE BLANK SUPPORT 2 3 5 5 ATTACHING THE BURETTE 2 3 5 6 CONNECTING PERISTALTIC PUMP TUBING 2 3 5 7 ELECTRICAL CONNECTIONS 2 3 2 4 2 5 2 6 2 6 2 8 2 9 2 11 2 4 2 4 2 5 2 6 2 7 2 8 2 10 ...

Page 26: ...2 2 ...

Page 27: ...um Protection Screen Electrodes Holder and Stirrer 1 pc Stirrer Holder Overhead Stirrer Propellers 3 pcs Support Rod Burette Blank Support 1 pc Pump and Burette Locking Screws with Plastic Head 2 pcs Temperature Sensor 1 pc Shorting Cap 1 pc Power Adapter 1 pc USB Cable 1 pc Instruction Manual 1 pc USB Memory Stick 1 pc HI900 PC Application Installation Kit on USB Stick 1 pc Quality Certificate 1 ...

Page 28: ...ce for more details 3 Always check that the titrant bottle and the titration beaker are on a flat surface 4 Always wipe up spills and splashes immediately 5 Avoid the following environmental working conditions Severe vibrations Direct sunlight Atmospheric relative humidity above 95 non condensing Environment temperatures below 10 C and above 40 C Explosion hazards 6 Have the titrator serviced only...

Page 29: ...2 5 SETUP 2 3 2 TITRATOR REAR VIEW 2 3 3 TITRATOR REAR VIEW WITH PERISTALTIC PUMP ...

Page 30: ...t be completed before connecting the Titrator to the power supply 2 3 5 1 ASSEMBLING STIRRER AND ELECTRODES HOLDER To assemble the electrode holder and support rod Remove protective cap from titrator case Insert the support rod into the titrator case and turn it clock wise to secure it in place ...

Page 31: ...er support housing can be inverted if necessary Insert electrode C temperature sensor D and stirrer E into the dedicated holes in the electrode holder Push them until they are in stable position Note For small sample sizes use the electrode adapter F in the center of the holder Slide the electrode holder into the support rod and set the desired height using the holder button ...

Page 32: ...into the titrator then slide it towards the front of the titrator case until it is firmly latched Secure the pump with the locking screw This procedure can be repeated to connect a second pump 2 3 5 4 ATTACHING BURETTE BLANK SUPPORT To attach the burette blank support follow these steps Insert burette blank support into the bay Lower the burette blank support into the titrator then slide it toward...

Page 33: ...TTE Make sure that the mark from the valve actuating cap and from the burette body are aligned While ensuring the correct coupling between the syringe plunger A and the pump piston B slide the burette into the support on the burette pump ...

Page 34: ...to the left side of the holder D The fitting on the top of the roller tube will sit in the top of the housing Manually rotate the pump A counter clock wise until the tubing it mounted on the pump Insert the roller tube B into the right side of the holder G The fitting on the top of the roller tube will sit in the top of the housing Attach aspiration and dispensing tubing to the roller tubing and r...

Page 35: ...tion Type of Connector A Connection for pH ORP ISE half cell and ISE combination electrodes BNC Socket B Reference electrode 4 mm Banana Socket C Temperature sensor RCA Socket D Stirrer 6 pin Connector E USB interface USB Standard B F Power input connector 24VDC DC Power Jack Connector G External PC keyboard 6 pin Mini DIN Standard PS2 H Printer DB 25 Socket I Extension interface 5 pin Connector J...

Page 36: ...2 12 ...

Page 37: ...ON KEYS 3 2 1 2 OPTION KEYS 3 2 1 3 ARROW KEYS 3 2 1 4 NUMERIC KEYS 3 2 1 5 ENTER KEY 3 2 2 DISPLAY 3 2 3 THE MAIN SCREEN 3 3 MENU NAVIGATION 3 3 1 SELECTING AN OPTION 3 3 2 SELECTING A MENU ITEM 3 3 3 ENTERING TEXT 3 3 4 SAVING MODIFICATIONS 3 3 3 4 3 4 3 5 3 5 3 7 3 7 3 8 3 4 3 4 3 5 3 5 3 6 3 7 3 7 ...

Page 38: ...3 2 ...

Page 39: ...he titrator from the power switch located on the back of the instrument Wait until the titrator finishes the initialization process Press when prompted or wait a few seconds for titrator to start Note All the performed initialization processes must be successfully completed If one of the initialization processes fails restart the titrator If the problem persists contact your nearest Hanna Service ...

Page 40: ...ssociated function is immediately performed Some of the keys are active only in specific screens Starts or Stops a titration Turns the selected stirrer On and Off Reserved Access the Data Parameters Menu reports GLP meter information report setup Displays Contextual Help 3 2 1 2 OPTION KEYS These keys are assigned to the virtual keys on the display Their functions are listed in the boxes above the...

Page 41: ...igate through menu options 3 2 1 4 NUMERIC KEYS Keys to Used for numeric entries Toggles between positive and negative values Decimal point 3 2 1 5 ENTER KEY This key has the following functions Accept alphanumeric data entry Executes the default underlined virtual option key 3 2 2 DISPLAY The titrator has a large color graphical display The main screen is shown below with short explanations of th...

Page 42: ...lected stirrer and actual set stirrer speed is displayed in RPM When stirrer is off the stirrer information is not displayed End point volume Displays the volume delivered to reach the titration end point When no titration has been performed the displayed volume is 0 000 mL Result Displays the titration result or the direct reading measurement mV or pH reading Displays the current readings The rea...

Page 43: ...ay a scroll bar is active on the right side The and keys can be used to scroll through the pages To activate the selected menu item press or 3 3 3 ENTERING TEXT To enter text in an alphanumeric input box first erase the previous text by using To enter a letter highlight it using the arrow keys then press Use the same procedure to enter the whole name For editing use the and keys When editing is co...

Page 44: ...om Saving Method screen without saving press or highlight the Exit Without Saving Method option and then press To save the modifications highlight the Save Method option and then press Note To access the contextual help menu press at any time Help is related to the displayed screen Press or to return to the previous screen ...

Page 45: ...TURE SETTING 4 4 3 TEMPERATURE UNITS 4 5 DATE AND TIME SETTING 4 6 DISPLAY SETTINGS 4 7 BEEPER 4 8 STIRRER 4 9 LANGUAGE 4 10 TOTAL VOLUME ALERT 4 11 TITRANT AGE REMINDER 4 12 USB LINK WITH PC 4 13 SETUP BALANCE INTERFACE 4 14 PRINTER MODE 4 15 RESET TO DEFAULT SETTINGS 4 16 OPTIMIZE MEMORY SPACE 4 17 UPDATE SOFTWARE 4 3 4 5 4 13 4 7 4 14 4 8 4 8 4 10 4 10 4 11 4 4 4 6 4 13 4 7 4 14 4 8 4 9 4 10 4 ...

Page 46: ...4 2 ...

Page 47: ...save files from the titrator to a USB storage device On the titrator the available file types are Standard Method Files HIXXXXYY MTD e g HI0001EN MTD HI1004EN MTD User Method Files USERXXXX MTD e g USER0001 MTD Report Files Ti_XXXXX RPT mV_XXXXX RPT pH_XXXXX RPT ISEXXXXX RPT mVrXXXXX RPT e g Ti_00001 RPT mV_00001 RPT pH_00001 RPT ISE00001 RPT mVr00001 RPT Use the and keys to select the file type T...

Page 48: ...leting Note The saved files will be stored on the USB key in the HI931 folder as follows Methods USB Drive HI931 Methods mtd Reports USB Drive HI931 Reports rpt 4 2 RESTORE FILES FROM USB STORAGE DEVICE This screen allows the user to transfer files from the USB storage device to the titrator Standard Method Files HIXXXXYY MTD e g HI0001EN MTD HI1004EN MTD User Method Files USERXXXX MTD e g USER000...

Page 49: ...e files from a USB key please ensure that the methods and or reports you wish to transfer to the titrator are in the correct folder Methods USB Drive HI931 Methods mtd Reports USB Drive HI931 Reports rpt 4 3 ADMINISTRATION A 4 digit numeric PIN can be set to prevent unauthorized changes from being made When the user enters administration and a pin has not been set the user will be prompted to ente...

Page 50: ...titrator can be unlocked by entering the PIN If the PIN is lost or forgotten press recovery pin and contact technical support to supply the required information 4 4 TEMPERATURE The Temperature Menu allows access to all of the settings related to temperature ...

Page 51: ...he temperature probe When Manual Temperature is selected Manual is displayed on the main screen and a preset temperature value is used for temperature compensation Note The selected temperature source will be indicated in the report files A for Automatic and M for Manual 4 4 2 MANUAL TEMPERATURE SETTING Option 5 0 to 105 0 C 23 0 to 221 0 F 268 2 to 378 2 K If the temperature probe is not connecte...

Page 52: ...s or the numeric keys to modify the date and time Press to move the cursor to the next field Press or to change the time format 4 6 DISPLAY SETTINGS This screen allows the user to customize the display settings Option Keys Increases the backlight saver time interval Decreases the backlight saver time interval The backlight intensity can be adjusted using and keys There are 8 levels of backlight in...

Page 53: ...ount of time If the display backlight is off any keystroke will activate the backlight without performing any action The range for the backlight saver timer is 1 to 60 minutes To disable the backlight saver increase the time to the maximum allowed The Off indication will appear 4 7 BEEPER Option On or Off If enabled on an audible alert will sound after a titration is completed when an invalid key ...

Page 54: ...pañol 4 10 TOTAL VOLUME ALERT Option Off 0 to 10000 mL This screen allows a programmable reminder to appear when the titrant reservoir is below 100 mL The titrant volume will decrease as the titrant is used After the new titrant volume has been entered in the Total Volume Alert screen a warning message appears on the main screen reminding the user re standardize the titrant ...

Page 55: ...rom the titrator to the PC Make sure that HI900 PC application is running on the PC Active Inactive shows the status of the USB link with the PC Active means that the titrator is using the USB communication with the PC and not with another device Ready shows that the titrator is able to communicate with the PC During transfer of any information between the PC and the titrator Transmit and informat...

Page 56: ...cted balance automatic weight acquisition will be not available Press to customize the name and serial communication parameters used by the selected balance Be sure that the settings on the titrator Balance Configuration menu match the settings for your particular balance baud rate data bits parity stop bits number request command syntax It may be necessary to change settings on your balance Users...

Page 57: ...i mode Use this mode when your printer is set as Ascii In this case only some of the accented characters symbols available in titrator will be printed on your printer Text mode Use this mode when you don t need to print the accented characters 4 15 RESET TO DEFAULT SETTINGS Note This will also delete all the user created methods and restore all manufacturer settings such as titrator configuration ...

Page 58: ...storage device containing a software setup kit To update the software Copy the Setup931 folder to a USB storage device Insert the USB storage device into the titrator Go to General Options then Update Software The titrator will display the current and new software versions Press When prompted remove the USB storage and restart the titrator ...

Page 59: ...END POINT MODE 5 5 6 1 FIXED END POINT pH OR mV 5 5 6 2 EQUIVALENCE END POINT pH OR mV 5 5 7 RECOGNITION OPTIONS EQUIVALENCE END POINT ONLY 5 5 7 1 THRESHOLD 5 5 7 2 RANGE 5 5 7 3 FILTERED DERIVATIVES 5 5 12 PRE TITRATION VOLUME 5 5 13 PRE TITRATION STIR TIME 5 5 10 MEASUREMENT MODE 5 5 10 1 SIGNAL STABILITY 5 5 10 2 TIMED INCREMENT 5 5 11 ELECTRODE TYPE 5 5 12 BLANK OPTION 5 5 13 CALCULATIONS 5 5...

Page 60: ... OPTION 5 5 15 TITRANT NAME 5 5 16 TITRANT CONCENTRATION 5 5 17 ANALYTE SIZE 5 5 18 ANALYTE ENTRY 5 5 18 1 FIXED WEIGHT OR VOLUME 5 5 18 2 MANUAL WEIGHT OR VOLUME 5 5 19 MAXIMUM TITRANT VOLUME 5 5 20 POTENTIAL RANGE 5 5 21 VOLUME FLOW RATE 5 5 22 SIGNAL AVERAGING 5 5 23 SIGNIFICANT FIGURES 5 6 PRINTING 5 24 5 32 5 26 5 33 5 29 5 30 5 30 5 31 5 31 5 25 5 33 5 27 5 29 5 30 5 31 5 31 5 32 ...

Page 61: ...evice 5 1 SELECTING METHODS To select a method press from the main screen A list of available methods will be displayed In the Analysis Methods screen you can view the list of all available methods standard and user methods To select a method highlight the method then press the name of the selected method will be displayed on the main screen 5 2 STANDARD METHODS The standard methods are developed ...

Page 62: ...thods from a PC using the HI900 PC application see General Options section 5 2 2 DELETING STANDARD METHODS Unnecessary standard methods can be removed from the titrator by following the procedure below From General Options Screen Using the and keys highlight the Save to USB Storage Device option and press Using the and keys navigate through the file types menu to find standard method files The ava...

Page 63: ...e deletion Press again to confirm or press to cancel the operation 5 3 USER METHODS These methods are defined by the user usually by modifying a standard method The user methods can be developed in accordance with the requirements of the user All method parameters can be modified by the user 5 3 1 CREATING USER METHODS To create a new user method start from a standard or user method and follow the...

Page 64: ...aracters 5 4 VIEW MODIFY METHOD To modify the method parameters press from the main screen A list of all the parameters for the selected method will be displayed Using the and keys highlight the option that you want to modify and choose To exit the View Modify Method screen press You can choose to save the modifications or to discard them ...

Page 65: ...5 7 TITRATION METHODS 5 5 2 METHOD REVISION Option Up to 3 characters 5 5 3 STIRRER CONFIGURATION Use the arrow keys to select the menu option 5 5 3 1 STIRRER Option Stirrer 1 or Disabled ...

Page 66: ...5 8 TITRATION METHODS 5 5 3 2 STIRRER SPEED Option 200 to 2500 RPM 5 5 4 PUMP CONFIGURATION Option Pump 1 or Pump 2 if installed ...

Page 67: ...specific applications Note For steep and normal titration curves smaller volume increments are recommended to obtain many points around the equivalence point For flat titration curves larger volume increments are recommended for equivalence point detection To set the dosing volume select Linear Dosing and enter the optimum dose Dosing volume ranges are 5 mL burette 0 001 to 4 750 mL 10 mL burette ...

Page 68: ...a and improved accuracy The following parameters must be set min Vol The smallest dose to be dispensed during a titration The min Vol must be greater than or equal to 0 001 mL for a 5 mL burette 0 001 mL for a 10 mL burette 0 005 mL for a 25 mL burette 0 005 mL for a 50 mL burette max Vol The largest dose to be dispensed during a titration The max Vol must be less than or equal to 4 000 mL delta E...

Page 69: ... 6 1 FIXED END POINT pH OR mV Fixed End Point pH Option 2 000 to 20 000 pH The titration is terminated when the preset pH value has been exceeded The end point volume is a calculated value based on the dispensed volume when pH is under the preset value and the dispensed volume when pH exceeded the preset value ...

Page 70: ...he same as for pH but the threshold value is expressed in mV 5 5 6 2 EQUIVALENCE END POINT pH OR mV The titration is terminated when the equivalence point is detected the point where the added quantity of titrant equals the quantity of analyte present in the sample Number of Equivalence Points Option 1 to 5 ...

Page 71: ...int volume is a calculated value based on a number of points around the equivalence point The potentiometric titration curve is the response in mV potential or pH between the indication of the electrode versus the volume of titrant added The inflection point of the titration curve is assumed to be the equivalence point of the chemical reaction For non symmetric titration curves the theoretical err...

Page 72: ... The first derivative must be greater than the threshold value at the maximum point see Recognition Options section 2nd Derivative When second derivative is used to recognize the equivalence point the titration curve inflection point EQP is the point where the second derivative crosses zero The detection algorithm looks for the point where the second derivative changes sign The checked point or fi...

Page 73: ... titrant sample species and concentrations and or electrode response 5 5 7 1 THRESHOLD Option 1 to 9999 mV mL This parameter must be set by the user according to the analysis The threshold represents the absolute value of the first derivative expressed in mV mL below which the detection algorithm does not search for the equivalence point The recommended value is 40 of the absolute value of the fir...

Page 74: ... mL Flat 1 to 450 Normal 50 to 1800 Steep 1800 to 9999 5 5 7 2 RANGE Option 2 000 to 20 000 pH or 2000 0 to 2000 0 mV Range is an optional feature for equivalence point recognition The titrator will only look for an equivalence point between the set values The Range option can be enabled by selecting Yes in the Range Options screen ...

Page 75: ...ltered Derivatives option can be enabled by selecting Yes in the Filtered Derivatives Option screen Noise can be due to Chemical system properties sample titrant solvent such as slow chemical reactions or unbuffered samples such as wastewater tap water wine Electrode response Incorrect method parameters settings such as Signal Stability Stirring Speed etc Insufficient titrant additions Note A shif...

Page 76: ...n volumes are shown below 0 001 to 4 750 mL for a 5 mL burette 0 001 to 9 500 mL for a 10 mL burette 0 005 to 23 750 mL for a 25 mL burette 0 005 to 47 500 mL for a 50 mL burette To disable a pre titration volume enter 0 000 mL Note A pre titration volume is highly recommended whenever possible Fewer doses will considerably shorten the overall titration duration 5 5 9 PRE TITRATION STIR TIME Optio...

Page 77: ...tor acquires the potential mV only when stable conditions are reached The principles of signal stability are plotted below The signal stability window condition represents the time interval t during which the potential measured in solution mV is confined inside the potential interval E The new signal value is acquired if the stability condition is reached after the minimum t min wait time If the s...

Page 78: ...om 2 seconds to t max wait time t max wait the maximum elapsed time between two successive doses If the t max wait has elapsed a new dose is added even if the signal stability condition is not reached The range is from t min wait time to 180 seconds 5 5 10 2 TIMED INCREMENT Option 2 to 180 seconds When timed increment is selected the titrator acquires the potential mV at a fixed time interval no s...

Page 79: ...cters 5 5 12 BLANK OPTION Option Disabled V Blank or Blank V This feature allows the user to select the procedure for the blank calculations where V is the volume of titrant dispensed during the titration and blank is the volume of titrant consumed by the blank sample ...

Page 80: ...nt volume titrant volume at the equivalence point or at the fixed end point and a formula selected by the user 5 5 13 1 STANDARD TITRATION 5 5 13 1 1 EDIT VARIABLE VALUES Edit the variables in a previously selected calculation For each formula selected variables can be changed 5 5 13 1 2 NO FORMULA mL ONLY Only the volume of titrant mL required to reach the end point will be displayed 5 5 13 1 3 N...

Page 81: ...rovide the results based on the titrant and sample units selected Titrant Units M mol L moles liter N eq L equivalents liter g L grams liter mg L milligrams liter Final Result Units ppt g kg parts per thousand grams kilogram ppm mg kg parts per million milligrams kilogram ppb µg kg parts per billion micrograms kilogram g 100 g percentage in weight grams 100 grams mg g milligrams gram mg kg milligr...

Page 82: ...trant used 5 5 13 1 5 SAMPLE CALCULATIONS BY VOLUME This calculation is used when the concentration of an analyte is determined in terms of the volume of sample The results are based on the initial sample volume in milliliters The titrator will calculate the results based on the selected units Titrant Units M mol L moles liter N eq L equivalents liter g L grams liter mg L milligrams liter ...

Page 83: ... L equivalents liter meq L milliequivalents liter A formula example is shown below using N eq L as the titrant units and g L as the final result units Variables can be set according to the amount of sample and titrant used 5 5 13 1 6 STANDARDIZE TITRANT BY WEIGHT This calculation is used when the concentration of the titrant is determined using a solid standard Determination of the titrant concent...

Page 84: ...tion of the titrant is determined using a primary standard solution Determination of the titrant concentration is based on the primary standard volume in milliliters The calculation is based on the selected titrant unit If the titrant unit is N eq L the formula used to calculate the result is displayed below ...

Page 85: ...ntage in weight grams 100 grams M mol L Molarity moles liter mg g milligrams gram N eq L Normality equivalents liter g L gram liter mg kg milligrams kilogram mg L milligrams liter mol kg moles kilogram µg L micrograms liter mol L moles liter mmol g millimoles gram eq kg equivalents kilogram mmol L millimoles liter meq kg milliequivalents kilogram mg mL milligrams milliliter mg 100 mL milligrams 10...

Page 86: ...s Liter mg L milligram Liter Reaction Ratio The reaction ratio is the ratio between the analyte and titrant or standard and titrant Examples of ratios mol mol moles of sample moles of titrant mol eq moles of sample equivalents of titrant eq mol equivalents of sample moles of titrant mol mol moles of titrant moles of standard eq mol equivalents of titrant moles of standard Example 2 moles of NaOH r...

Page 87: ...culations can be used The calculations are based on the original sample weight volume in order to express the results for the initial sample Final Dilution Volume The volume of the sample after dilution Aliquot Volume Volume of sample taken from the dilution for titration Analyte size to be diluted The initial sample weight volume 5 5 15 TITRANT NAME Option Up to 15 characters ...

Page 88: ...e used When determining the titrant concentration only the concentration unit is displayed 5 5 17 ANALYTE SIZE Option 0 001 to 250 0 Enter the size of the sample for sample concentration determinations or standard for titrant concentration determination 5 5 18 ANALYTE ENTRY Option Fixed or Manual ...

Page 89: ...in the titration must be set according to the analysis If the titration end point fixed or equivalence End Point is not reached the titration will be terminated after the maximum titrant volume has been dispensed The error message Limits Exceeded will appear on the display 5 5 20 POTENTIAL RANGE Option 2000 0 to 2000 0 mV The input potential range can be set by the user The titration will be termi...

Page 90: ... burette size and display the correct high limit volume The flow rate is set for all burette operations 5 5 22 SIGNAL AVERAGING Option 1 2 3 or 4 readings This option enables filtering on the mV pH reading If 1 Reading is selected the filtering is disabled The titrator will take the last reading and place it into a moving window along with the last 2 3 or 4 readings depending on the selected optio...

Page 91: ... titration result 5 6 PRINTING To print method parameters press from the main screen Press and wait a few seconds until the printer completes the job If no printer is connected to the dedicated socket or if the printer is offline an error message will appear on the display see Connecting a Printer section for information about connecting a printer to the titrator ...

Page 92: ...5 34 ...

Page 93: ...6 1 TITRATION MODE CHAPTER 6 TITRATION MODE 6 1 RUNNING A TITRATION 6 1 1 STARTING A TITRATION 6 1 2 SUSPENDING A TITRATION 6 1 3 VIEWING THE TITRATION CURVE 6 2 STOPPING A TITRATION 6 3 6 3 6 5 6 3 6 3 ...

Page 94: ...6 2 ...

Page 95: ...tration stir time starts if enabled see Titration Methods section After the pre titration stir time is complete the pre titration volume will be displayed if enabled see Titration Methods section The titrator will start the analysis and continue to deliver titrant until the end point is detected or the titration is terminated 6 1 2 SUSPENDING A TITRATION While a titration is in progress you can te...

Page 96: ...f titrant are displayed see Figure 2 Fixed End Point pH The pH readings vs volume of titrant are displayed see Figure 3 Fixed End Point mV The mV readings vs volume of titrant are displayed see Figure 4 Changes the y axis scale to either the mV or pH readings or the selected derivative values of mV or pH Available only for titrations with equivalence end points Allows you to save the graph as a bi...

Page 97: ...nt titration terminated by the user before the end point was detected Limits Exceeded The maximum titrant volume was delivered without reaching the end point An error message is displayed on the screen Critical Error A critical error occurred and the titration was stopped These errors are typically related to the dosing system An error message is displayed on the screen Potential Out of Range The ...

Page 98: ...6 6 ...

Page 99: ... CALIBRATION REMINDER 7 2 6 SET REMINDER PERIOD 7 2 7 CLEAR CALIBRATION 7 2 8 pH GLP DATA 7 2 9 LOGGING INTERVAL 7 2 10 STABILITY CRITERIA 7 2 11 pH RESOLUTION 7 2 12 STIRRER CONFIGURATION 7 2 13 STIRRING SPEED 7 3 pH CALIBRATION 7 4 LOGGING 7 4 1 INTERVAL LOGGING 7 4 2 MANUAL LOGGING 7 3 7 4 7 12 7 5 7 13 7 7 7 8 7 8 7 9 7 10 7 4 7 5 7 13 7 6 7 7 7 8 7 9 7 9 7 10 ...

Page 100: ...7 2 ...

Page 101: ...ccess to options that are not directly related to the measurement process see General Options section Stores the current pH reading see Manual Logging section or Starts the interval log see Automatic Logging section Enter the pH calibration screen see pH Calibration section Enter the pH setup screen parameters are associated with pH measurements and calibration see pH Setup section Allow the user ...

Page 102: ... Automatic The instrument automatically selects the pH calibration point as the closest buffer from the predefined buffer group see Edit Buffer Group section Semiautomatic The instrument automatically selects the closest buffer from the available buffers standard and custom buffers Manual The calibration buffer must be manually selected by the user during calibration from the available buffer list...

Page 103: ...ill not be changed 7 2 3 EDIT CUSTOM BUFFERS If you wish to use buffers other than the standard ones use the Edit Custom Buffers option to set the desired pH value up to five pH custom buffers can be set Note Custom buffers are not temperature compensated enter the value of the buffer at the calibration temperature Use and keys to select the desired buffer Press to delete the selected buffer Press...

Page 104: ...om to be used for automatic buffer recognition Within the buffer group pH values must be at least 1 5 pH far apart If the buffer group already contains five pH buffers at least one pH buffer has to be removed in order to add another buffer Use the arrow keys to select the pH buffer to be included removed in from the buffer group Press or to add remove the selected pH buffer to from buffer group Pr...

Page 105: ...ation reminder will not appear 7 2 6 SET REMINDER PERIOD If Daily or Periodic option was selected for the calibration reminder the reminder period must also be set For a daily reminder period the time of day can be set For a periodic reminder period the number of days hours and minutes can be set Press to move the cursor to the next field Press to save the changes or to return to the previous scre...

Page 106: ...n is cleared the factory calibration will be used Press to clear the previous calibration or to return to the previous screen without clearing the calibration 7 2 8 pH GLP DATA Displays the pH calibration data 7 2 9 LOGGING INTERVAL Option 2 seconds to 8h 59 min 59 sec Set the logging interval to be used for automatic logging ...

Page 107: ... stability criteria Fast Quicker results with less accuracy Medium Medium speed results with medium accuracy Accurate Slower results with high accuracy 7 2 11 pH RESOLUTION Option One X X Two X XX or Three X XXX decimal places 7 2 12 STIRRER CONFIGURATION Option Stirrer 1 or Disabled ...

Page 108: ...librate the instrument often especially if high accuracy is required The instrument should be recalibrated Whenever the pH electrode is replaced At least once a week After testing aggressive chemicals When No pH Calibration or pH Calibration Expired message appears on the display ...

Page 109: ...is suggested For pH titrations the selected buffers should bracket your end point e g if your end point value is at 8 5 use 7 01 or 6 86 and 9 18 or 10 01 for calibration To begin calibration Press If the instrument was calibrated before the old calibration can be cleared by pressing Note It is very important to clear calibration history when a new electrode is used Immerse the pH electrode and th...

Page 110: ...trode or check the buffer Press to update calibration This message alerts the user that some dirt or deposits could be on the electrode or the buffer is contaminated Slope too low Please check the buffer This message appears if the current slope is under 80 of the default slope Recalibrate the instrument using fresh buffers Slope too high Press to clear the old calibration This message appears as ...

Page 111: ...to start the log The logging interval and name of logging file will be displayed on the pH measurement screen To stop the automatic logging press 7 4 2 MANUAL LOGGING To manually log pH readings press from the pH measurement screen A new record will be added to the report every time is pressed ...

Page 112: ...7 14 ...

Page 113: ... 8 2 1 CLEAR RELATIVE mV OFFSET 8 2 2 LOGGING INTERVAL 8 2 3 STABILITY CRITERIA 8 2 4 STIRRER CONFIGURATION 8 2 5 STIRRING SPEED 8 3 RELATIVE mV CALIBRATION 8 4 LOGGING 8 4 1 INTERVAL LOGGING 8 4 2 MANUAL LOGGING 8 3 8 4 8 5 8 5 8 6 8 7 8 4 8 4 8 5 8 6 8 7 ...

Page 114: ...8 2 ...

Page 115: ...creen gives access to options that are not directly related to the measurement process see General Options section Stores the current mV reading see Manual Logging section or Starts the mV interval log see Automatic Logging section Enter the mV calibration screen see pH Calibration section Enter the mV setup screen parameters are associated with pH measurements and calibration see pH Setup section...

Page 116: ...8 4 mV MODE 8 2 mV SETUP 8 2 1 CLEAR RELATIVE mV OFFSET Press to clear the relative mV offset or to return to the previous screen 8 2 2 LOGGING INTERVAL Option 2 seconds to 8h 59min 59sec ...

Page 117: ...Medium or Accurate Fast Quicker results with less accuracy Medium Medium speed results with medium accuracy Accurate Slower results with high accuracy 8 2 4 STIRRER CONFIGURATION Option Stirrer 1 or Disabled 8 2 5 STIRRING SPEED Option 200 to 2500 RPM ...

Page 118: ...tically Interval Logging at predefined time intervals To customize the logging report Press to display the Data Parameters screen Highlight the Setup pH mV ISE Report option and press to display the Setup pH mV ISE Report screen Use the and keys to highlight the data field that you want to show hide in the pH mV ISE report and then press to activate deactivate it Each field marked by is an active ...

Page 119: ...to start the log The logging interval and name of logging file will be displayed on the measure screen To stop the automatic logging press again 8 4 2 MANUAL LOGGING To manually log mV readings press from the mV measurement screen A new record will be added to the report every time is pressed ...

Page 120: ...8 8 ...

Page 121: ...9 2 7 SET REMINDER PERIOD 9 2 8 CLEAR CALIBRATION 9 2 9 ISE GLP DATA 9 2 10 ELECTRODE TYPE 9 2 11 CONCENTRATION UNIT 9 2 12 LOGGING INTERVAL 9 2 13 STABILITY CRITERIA 9 2 14 ISE SIGNIFICANT DIGITS 9 2 15 STIRRER CONFIGURATION 9 2 16 STIRRING SPEED 9 3 ISE CALIBRATION 9 4 LOGGING 9 4 1 INTERVAL LOGGING 9 4 2 MANUAL LOGGING 9 3 9 4 9 11 9 5 9 11 9 6 9 13 9 7 9 8 9 9 9 10 9 4 9 4 9 11 9 5 9 12 9 13 9...

Page 122: ...9 2 ...

Page 123: ...ns screen gives access to options that are not directly related to the measurement process see General Options section Stores the current concentration reading see Manual Logging section or Starts the ISE interval log see Interval Logging section Enter the ISE calibration screen see ISE Calibration section Enter the ISE setup screen Parameters are associated with ISE measurements and calibration A...

Page 124: ...roup All Standards The set of available standards includes the Standard solutions and Custom solutions Standards Group The set of available standards includes only the standards selected by the user 9 2 2 TEMPERATURE COMPENSATION Option Enabled or Disabled Note If you enabled Temperature Compensation then the isopotential point must be set ...

Page 125: ...bled The isopotential point is edited in ppm units only The isopotential point will vary for different electrodes if measurements are going to be made at several temperatures the value should be entered if it is known 9 2 4 EDIT CUSTOM STANDARDS Option Up to five Use the and keys to select the standard Press to delete the standard Press to edit the selected custom standard use the numeric keys to ...

Page 126: ...add remove the selected standard to from standard group Press to return to ISE Setup menu 9 2 6 CALIBRATION REMINDER Option Daily Periodic or Disabled Daily The calibration reminder will appear daily at specified time Periodic The calibration reminder will appear after the set time has elapsed since the last calibration Disable The calibration reminder will not appear ...

Page 127: ...days hours and minutes can be set Press to move the cursor to the next field Press to save the changes or to return to the previous screen Press to disable the calibration reminder and return to ISE setup menu 9 2 8 CLEAR CALIBRATION This option clears the existing ISE calibration If the calibration is cleared a new calibration must be done in order to take measurements Press to clear the previous...

Page 128: ...ion Ammonia Bromide Cadmium Calcium Carbon Dioxide Chloride Cupric Cyanide Fluoride Iodide Lead Nitrate Potassium Silver Sodium Sulfate Sulfide or five custom electrodes For Standard ISE Press to see the ion constants name molar weight electric charge slope press to return to the setup screen ...

Page 129: ...Molecular Weight in g mol using the numeric keys Press to save the value or press to return to the previous screen Select the appropriate Electric Charge Slope Use the and keys to select the value and then press If the electric charge is none manually set the slope by pressing Press to save the value or press to return to the previous screen 9 2 11 CONCENTRATION UNIT Options ppt g L ppm mg L ppb µ...

Page 130: ...59 min 59 sec 9 2 13 STABILITY CRITERIA Option Fast Medium Accurate Fast Quicker results with less accuracy Medium Medium speed results with medium accuracy Accurate Slower results with high accuracy 9 2 14 ISE SIGNIFICANT DIGITS Option One X Two XX or Three XXX ...

Page 131: ...he standard solution into clean beakers If possible use plastic beakers to minimize any EMC interferences For accurate calibration and to minimize cross contamination use two beakers for each standard solution one for rinsing the electrode and one for calibration Note For accurate measurements add the appropriate ISA Ionic Strength Adjustment to the calibration standards CALIBRATION PROCEDURE Befo...

Page 132: ...t and repeat the procedure with all of the available standards Press to exit the calibration 9 4 LOGGING Data logging is available in ISE mode It can be logging on demand Manual Logging or automatically Interval Logging at predefined time intervals To customize the logging report Press to display the Data Parameters screen Highlight the Setup pH mV ISE Report option and press to display the Setup ...

Page 133: ... Press to start the log The logging interval and name of logging file will be displayed on the measure screen To stop the automatic logging press again 9 4 2 MANUAL LOGGING To manually log ISE readings press from the ISE screen A new record will be added to the report every time is pressed ...

Page 134: ...9 14 ...

Page 135: ...IP 10 1 3 MANUAL DISPENSE 10 1 4 PURGE BURETTE 10 2 STIRRER 10 3 RESULTS 10 3 1 REVIEW LAST ANALYSIS REPORT 10 3 1 REVIEW AVAILABLE REPORTS 10 3 1 GLP DATA 10 3 1 METER INFORMATION 10 3 1 SETUP pH mV ISE REPORT 10 3 1 SETUP TITRATION REPORT 10 3 10 4 10 5 10 6 10 7 10 8 10 9 10 3 10 4 10 6 10 6 10 7 10 9 ...

Page 136: ...10 2 ...

Page 137: ... active if two pumps are connected 10 1 1 PRIME BURETTE Option Up to 5 The Prime Burette option is used to fill the burette with titrant or reagent before starting a titration The priming process consists of several cycles of filling and emptying the burette with titrant Two rinse cycles of burette are shown in the figure below The dispensing tube is connected on the right side and the aspiration ...

Page 138: ...lect Prime Burette enter the number of rinses and press We recommend at least three rinses to assure that the air bubbles are completely removed 10 1 2 RINSE TIP A 2 mL dose of titrant will be dispensed from the burette when this operation is selected this will eliminate any air in the dispensing tip 10 1 3 MANUAL DISPENSE Manual Dispense option allows a defined titrant volume to be dosed Select t...

Page 139: ...o 9 500 mL for a 10 mL burette 0 005 to 23 750 mL for a 25 mL burette 0 005 to 47 500 mL for a 50 mL burette 10 1 4 PURGE BURETTE This option allows the burette to be emptied before cleaning and or storing the burette The burette is flushed twice Note Before starting this operation remove the aspiration tube from the titrant bottle The figures below show the steps in a purge burette operation ...

Page 140: ...From the Data Parameters screen you can access the following options 10 3 1 REVIEW LAST ANALYSIS REPORT The information seen in the report is based on the selections made in the Setup Titration Report and Setup ISE pH mV Report screen The following option keys are available Review the graph Print the titration report Return to the previous screen Keys can be used to scroll through the pages ...

Page 141: ...press The report contains only the information selected in the Setup Titration Report and Setup pH mV ISE Report screens during report configuration The following option keys are available Review the selected graph Review the selected report Print the selected report Delete the selected report Return to the previous screen 10 3 3 GLP DATA Option Up to 20 characters ...

Page 142: ...itration report 10 3 4 METER INFORMATION Displays titrator configuration data Titrator Serial Number The serial number of the titrator base board Analog Board 1 Serial Number The serial number of the analog board Pump 1 and or 2 Serial Number The serial number of the connected pump Titrator Software Version The current software version installed on the titrator Base Board Software Version The curr...

Page 143: ...d Update the report with the select items Report previously saved will not be updated Scroll through the options 10 3 6 SETUP TITRATION REPORT Customize a unique report to record the titration results An asterisk means that it will be included in the titration report Adds the highlighted information to the report Removes the highlighted information from the report Returns to the Data Parameter Scr...

Page 144: ...10 10 ...

Page 145: ...G THE BURETTE 11 1 3 DISASSEMBLING THE BURETTE 11 1 4 ASSEMBLING THE BURETTE 11 1 5 CLEANING THE BURETTE 11 1 6 BURETTE PREPARATION FILLING WITH TITRANT 11 2 PERIPHERALS 11 2 1 CONNECTING TO A PRINTER 11 2 2 CONNECTING AN EXTERNAL PC KEYBOARD 11 2 3 CONNECTING TO A COMPUTER 11 3 11 3 11 4 11 5 11 6 11 8 11 3 11 3 11 4 11 6 11 6 ...

Page 146: ...11 2 ...

Page 147: ...HE BURETTE Remove the burette from the pump assembly by sliding it forward and then slide the new burette into place 11 1 3 DISASSEMBLING THE BURETTE The aspiration and the dispensing tubes have fittings and tube protectors The aspiration tube is mounted in the left side and the dispensing tube is mounted in the right side of the burette To remove the dispensing tube and the aspiration tube follow...

Page 148: ... fill the burette use 2 rinses see Auxiliary Functions chapter During second cycle remove the aspiration tube from the cleaning solution deionized water or solvent and allow the air to replace the liquid in the burette This will clean the aspiration tube If this simple cleaning procedure is not adequate continue with these steps Remove the burette assembly from the pump Remove the dispensing and a...

Page 149: ...ations If necessary clean the burette and make sure it is empty From the main screen press Highlight Prime Burette option and press Enter the number of times the burette needs to be rinsed minimum three rinses are recommend allowing air bubbles to be evacuated Press To avoid the presence of the air bubbles inside the burette make sure to have a continuous liquid flow inside the burette A little ai...

Page 150: ... turned off 11 2 1 CONNECTING TO A PRINTER A variety of parallel printers can be connected to the parallel port of the titrator using a DB25 cable Warning The titrator and the external printer must be both turned OFF before they are connected 11 2 2 CONNECTING AN EXTERNAL PC KEYBOARD This connection allows you to use an external PS 2 PC Keyboard in addition to the titrator s keypad ...

Page 151: ...F 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 Enter Alphanumer...

Page 152: ...e PC Connect the cable to the USB port on the rear panel of the titrator Connect the cable to the USB port on the PC Open the USB Communication screen on the titrator see General Options chapter Launch the HI900 PC application and then select the appropriate USB Port on the PC The HI900 PC application allows the transfer of methods and reports between the titrator and PC ...

Page 153: ...A1 1 TECHNICAL SPECIFICATIONS APPENDIX 1 TECHNICAL SPECIFICATIONS A1 HI931 TECHNICAL SPECIFICATIONS A1 3 ...

Page 154: ...A1 2 ...

Page 155: ...urette 0 050 mL 50 mL Burette Stirrer Range 200 to 2500 RPM Resolution 100 RPM mV Range 2000 0 to 2000 0 mV Resolution 0 1 mV Accuracy 0 1 mV Calibration Single point offset pH Range 2 000 to 20 000 pH Resolution 0 1 0 01 0 001 pH Accuracy 0 001 pH Calibration Up to 5 points with standard or custom buffers ISE Range 1x10 6 to 9 999x1010 Resolution 1 0 1 0 01 Accuracy 0 001 pH Calibration Up to 5 p...

Page 156: ... drive Additional Specifications Electrode Holder 4 x multi purpose slots titrant reagent tubes 3 x 12 mm electrode slots 1 x temperature sensor slot 1 x overhead stirrer slot Display 5 7 graphical color display with backlight Languages English Portuguese Spanish Power Supply 100 240 Vac 50 60 Hz Power Draw 0 5 Amps Enclosure Material ABS PC and Stainless Steel Keypad Polyester Dimensions 315 x 20...

Page 157: ...TIONS IN FDA APPROVED BOTTLE A2 1 9 ELECTRODE REFILL ELECTROLYTE SOLUTIONS A2 1 10 ELECTRODE REFILL ELECTROLYTE SOLUTIONS IN FDA APPROVED BOTTLE A2 1 11 ORP PRETREATMENT SOLUTIONS A2 1 12 TITRATION REAGENTS A2 1 13 ION SELECTIVE ELECTRODE CALIBRATION STANDARDS A2 2 SENSORS A2 1 1 pH ELECTRODES A2 1 2 ORP ELECTRODES A2 1 3 HALF CELL ELECTRODES A2 1 4 ION SELECTIVE ELECTRODES A2 1 5 TEMPERATURE SENS...

Page 158: ...A2 2 ...

Page 159: ... Buffer Solution 500 mL HI8007L pH 7 01 Buffer Solution 500 mL HI8009L pH 9 18 Buffer Solution 500 mL HI8010L pH 10 01 Buffer Solution 500 mL A2 1 3 pH TECHNICAL CALIBRATION BUFFERS HI5016 pH 1 68 Buffer Solution 500 mL HI5003 pH 3 00 Buffer Solution 500 mL HI5004 pH 4 01 Buffer Solution 500 mL HI5068 pH 6 86 Buffer Solution 500 mL HI5007 pH 7 01 Buffer Solution 500 mL HI5091 pH 9 18 Buffer Soluti...

Page 160: ...t Cleaning Solution 500 mL A2 1 6 ELECTRODE CLEANING SOLUTIONS IN FDA APPROVED BOTTLE HI8061M General Purpose Solution 230 mL HI8061L General Purpose Solution 500 mL HI8073M Protein Cleaning Solution 230 mL HI8073L Protein Cleaning Solution 500 mL HI8077M Oil Fat Cleaning Solution 230 mL HI8077L Oil Fat Cleaning Solution 500 mL A2 1 7 ELECTRODE STORAGE SOLUTIONS HI70300M Storage Solution 230 mL HI...

Page 161: ...e Titration Reagent 1 L HI70448 0 02 M AgNO3 Titration Reagent 1 L HI70449 0 02 M EDTA Titration Reagent 1 L HI70455 0 01 N NaOH Titration Reagent 1 L HI70456 0 1 N NaOH Titration Reagent 1 L HI70457 1 N NaOH Titration Reagent 1 L HI70458 0 01 M H2 SO4 Titration Reagent 1 L HI70459 0 05 M H2 SO4 Titration Reagent 1 L HI70462 0 01 N HCl Titration Reagent 1 L HI70463 0 1 N HCl Titration Reagent 1 L ...

Page 162: ...pe refillable combination pH electrode Use emulsions fats and creams soil and semi solids samples HI1083B Glass body micro Viscolene nonrefillable combination pH electrode Use biotechnology and micro titration HI1131B Glass body double junction refillable combination pH electrode Use general purpose HI1330B Glass body semimicro single junction refillable combination pH electrode Use laboratory via...

Page 163: ...lurry forms of food HI1413B Glass body single junction flat tip non refillable Viscolene electrolyte combination pH electrode Use surfaces skin leather paper and emulsions A2 2 2 ORP ELECTRODES HI3131B Glass body refillable combination platinum ORP electrode Use laboratories and general purpose HI3230B Plastic body PEI gel filled combination platinum ORP electrode Use municipal water and quality c...

Page 164: ... HI4102 Bromide ISE HI4003 HI4103 Cadmium ISE HI4004 HI4104 Chloride ISE HI4105 Carbon Dioxide ISE HI4007 HI4107 Chloride ISE HI4008 HI4108 Cupric ISE HI4009 HI4109 Cyanide ISE HI4010 HI4110 Fluoride ISE HI4011 HI4111 Iodide ISE HI4012 HI4112 Lead ISE HI4013 HI4113 Nitrate ISE HI4014 HI4114 Potassium ISE HI4015 HI4115 Silver Sulfide ISE FC300B Sodium A2 2 5 TEMPERATURE SENSOR HI7662 TW Temperature...

Page 165: ...verhead Stirrer 3 propellers HI930301 Replacement Propellers 3 pcs HI930302 High Chemical Resistance Propellers 3 pcs HI930303 Stirrer Support HI930320 Pump Assembly HI930100 Pump Assembly with Peristaltic Pump HI930101 3 Way Valve HI900260 Tool for burette cap removal HI900942 Burette with 5 mL syringe HI930105 10 mL syringe HI930110 25 mL syringe HI930125 50 mL syringe HI930150 5 mL Syringe HI90...

Page 166: ...USA Plug HI900946 Temperature Probe HI7662 TW Power Adapter European Plug HI900947 Blank Support HI930191 Electrode adapter for overhead stirrer holder HI930311 Blank Burette Support HI930190 Replacement Cap and Rotor for Peristaltic Pump HI930201 Overhead Electrode Holder HI930310 Roller Tube for Titrator peristaltic pump 3 pcs HI930204 ...

Page 167: ...te collection point for the recycling of electrical and electronic equipment which will conserve natural resources Ensuring proper product and battery disposal prevents potential negative consequences for the environment and human health For more information contact your city your local household waste disposal service the place of purchase or go to www hannainst com Certification MAN931 10 18 ...

Page 168: ...he problem If the repair is not covered by the warranty you will be notified of the charges incurred If the instrument is to be returned to Hanna Instruments first obtain a Returned Goods Authorization RGA numberfromtheTechnical Service department and then send it with shipping costs prepaid When shipping any instrument make sure it is properly packed for complete protection Warranty Before using ...

Page 169: ...GENERAL TITRATION APPLICATIONS BROCHURE AUTOMATIC POTENTIOMETRIC TITRATOR HI931 ...

Page 170: ......

Page 171: ... is on the bottom of the beaker Record the exact weight of the sample once the balance has stabilized with an accuracy of 0 0001 grams Remove the beaker from the balance and add deionized water to the 50 mL mark on the beaker ANALYSIS Place the beaker under the stirrer assembly and lower it to immerse the pH electrode temperature probe and stirrer Ensure that the reference junction of the pH elect...

Page 172: ...sec Electrode Type pH Blank Option No Blank Calculations Stdz Titrant by Weight Dilution Option Disabled Titrant Name 0 1N NaOH Analyte Size 0 20000 g Analyte Entry Manual Maximum Titrant Volume 15 000 mL Potential Range 2000 0 to 2000 0 mV Volume Flow Rate 25 mL 50 0 mL min Signal Averaging 1 Reading Significant Figures XXXXX CALCULATIONS Calculations Stdz Titrant by Weight Titrant units N eq L T...

Page 173: ...using pH 4 01 7 01 and 10 01 buffers Refer to the instruction manual for calibration procedure SAMPLE PREPARATION Use a Class A volumetric pipette to transfer exactly 10 00 mL of 0 1N sodium hydroxide HI70456 to a clean 100 mL beaker Add deionized water to the 50 mL mark on the beaker ANALYSIS Place the beaker under the stirrer assembly and lower it to immerse the pH electrode temperature probe an...

Page 174: ...ec Max wait 15 sec Electrode Type pH Blank Option No Blank Calculations Stdz Titrant by Volume Dilution Option Disabled Titrant Name 0 1N HCl Analyte Size 10 0000 mL Analyte Entry Fixed Maximum Titrant Volume 15 000 mL Potential Range 2000 0 to 2000 0 mV Volume Flow Rate 25 mL 50 0 mL min Signal Averaging 1 Reading Significant Figures XXXXX CALCULATIONS Calculations Stdz Titrant by Volume Titrant ...

Page 175: ... of 0 0001 grams Carefully transfer the salt to a 100 mL Class A volumetric flask Add approximately 80 mL of deionized water and mix to dissolve Once the salt is completely dissolved bring the flask to volume with deionized water mix well Use a Class A volumetric pipette to transfer exactly 10 00 mL of the solution to a clean 100 mL plastic beaker Add deionized water to the 50 mL mark on the beake...

Page 176: ...y Weight Dilution Option Enabled Final Dilution Volume 100 000 mL Aliquot Volume 10 000 mL Titrant Name 0 1M Na2S2O3 Analyte Size 0 35000 g Analyte Entry Manual Maximum Titrant Volume 15 000 mL Potential Range 2000 0 to 2000 0 mV Volume Flow Rate 25 mL 50 0 mL min Signal Averaging 1 Reading Significant Figures XXXXX CALCULATIONS Calculations Stdz Titrant by Weight Titrant units M mol L Titrant vol...

Page 177: ...it for 2 hours at 150 C Cool to room temperature in a desiccator Carefully weigh approximately 0 49 grams of dried potassium dichromate Record the exact weight of the sample once the balance has stabilized with an accuracy of 0 0001 grams Carefully transfer the salt to a 100 mL Class A volumetric flask Add approximately 80 mL of deionized water and mix to dissolve Once the salt is completely disso...

Page 178: ... Stdz Titrant by Weight Dilution Option Enabled Final Dilution Volume 100 000 mL Aliquot Volume 10 000 mL Titrant Name 0 1M FAS Analyte Size 0 49000 g Analyte Entry Manual Maximum Titrant Volume 15 000 mL Potential Range 2000 0 to 2000 0 mV Volume Flow Rate 25 mL 50 0 mL min Signal Averaging 1 Reading Significant Figures XXXXX CALCULATIONS Calculations Stdz Titrant by Weight Titrant units M mol L ...

Page 179: ... mL volumetric flask Add approximately 80 mL of distilled water and mix Dissolve completely before bringing to volume Use a Class A volumetric pipette to transfer exactly 5 00 mL of prepared standard solution to a 150 mL glass beaker and add distilled water to the 100 mL mark on the beaker Add 10 00 mL of 1 5M nitric acid HI70427 to the beaker ANALYSIS Place the beaker under the stirrer assembly a...

Page 180: ...rant by Weight Dilution Option Enabled Final Dilution Volume 100 000 mL Aliquot Volume 5 000 mL Titrant Name 0 02M AgNO3 Analyte Size 0 20000 g Analyte Entry Manual Maximum Titrant Volume 15 000 mL Potential Range 2000 0 to 2000 0 mV Volume Flow Rate 25 mL 50 0 mL min Signal Averaging 1 Reading Significant Figures XXXXX CALCULATIONS Calculations Stdz Titrant by Weight Titrant units M mol L Titrant...

Page 181: ...ing If necessary prime the burette until all the air has been removed completely For the determination of the exact concentration of the 0 1N hydrochloric acid follow HI0002EN 0 1N Hydrochloric Acid Titrant Concentration Press from the main screen Use the arrow keys to highlight Alkalinity of Water and press ELECTRODE PREPARATION Press from the main screen if necessary select the analog board and ...

Page 182: ...Dilution Option Disabled Titrant Name 0 1N HCl Titrant Conc 0 1000 N eq L Analyte Size 50 000 mL Analyte Entry Fixed Maximum Titrant Volume 25 000 mL Potential Range 2000 0 to 2000 0 mV Volume Flow Rate 25 mL 50 0 mL min Signal Averaging 1 Reading Significant Figures XXXXX CALCULATIONS Calculations Sample Calc by Volume Titrant units N eq L Titrant volume dosed V L Final result units mg L Titrant ...

Page 183: ... necessary prime the burette until all the air has been removed completely For the determination of the exact concentration of the 0 1N sodium hydroxide follow HI0001EN 0 1N Sodium Hydroxide Titrant Concentration Press from the main screen Use the arrow keys to highlight Acidity of Water and press ELECTRODE PREPARATION Press from the main screen if necessary select the analog board and press Calib...

Page 184: ...tion Option Disabled Titrant Name 0 1N NaOH Titrant Conc 0 1000 N eq L Analyte Size 50 000 mL Analyte Entry Fixed Maximum Titrant Volume 25 000 mL Potential Range 2000 0 to 2000 0 mV Volume Flow Rate 25 mL 50 0 mL min Signal Averaging 1 Reading Significant Figures XXXXX CALCULATIONS Calculations Sample Calc by Volume Titrant units N eq L Titrant volume dosed V L Final result units mg L Titrant Con...

Page 185: ... of the exact concentration of the 0 02M Silver Nitrate follow HI0200EN 0 02M Silver Nitrate Titrant Concentration Press from the main screen Use the arrow keys to highlight HI1007EN Chloride in Water and press ELECTRODE PREPARATION Prepare the Silver Sulfide electrode according to the procedure in the manual SAMPLE PREPARATION Use a class A volumetric pipette to transfer exactly 100 00 mL of samp...

Page 186: ... Calculations Sample Calc by Volume Dilution Option Disabled Titrant Name 0 02M AgNO3 Titrant Conc 2 0000E 2 M mol L Analyte Size 100 0000 mL Analyte Entry Manual Maximum Titrant Volume 25 000 mL Potential Range 2000 0 to 2000 0 mV Volume Flow Rate 25 mL 50 0 mL min Signal Averaging 1 Reading Significant Figures XXXXX CALCULATIONS Calculations Sample Calc by Volume Titrant units M mol L Titrant vo...

Page 187: ...he exact concentration of the 0 05M sulfuric acid follow HI0103EN 0 05M Sulfuric Acid Titrant Concentration Press from the main screen Use the arrow keys to highlight HI1008EN Neutralization w H2SO4 and press ELECTRODE PREPARATION Press from the main screen if necessary select the analog board and press Calibrate the electrode using pH 4 01 7 01 and 10 01 buffers Refer to the instruction manual fo...

Page 188: ...n No Blank Calculations Sample Calc by Volume Dilution Option Disabled Titrant Name 0 05M H2S04 Titrant Conc 5 0000E 2 M mol L Analyte Size 10 000 mL Analyte Entry Fixed Maximum Titrant Volume 20 000 mL Potential Range 2000 0 to 2000 0 mV Volume Flow Rate 25 mL 50 0 mL min Signal Averaging 1 Reading Significant Figures XXXXX CALCULATIONS Calculations Sample Calc by Volume Titrant units M mol L Tit...

Page 189: ...ation of the exact concentration of the 0 1N sodium hydroxide follow HI0001EN 0 1N Sodium Hydroxide Titrant Concentration Press from the main screen Use the arrow keys to highlight HI1009EN Neutralization w NaOH and press ELECTRODE PREPARATION Press from the main screen if necessary select the analog board and press Calibrate the electrode using pH 4 01 7 01 and 10 01 buffers Refer to the instruct...

Page 190: ...ode Type pH Blank Option No Blank Calculations Sample Calc by Volume Dilution Option Disabled Titrant Name 0 1N NaOH Titrant Conc 0 1000 N eq L Analyte Size 10 000 mL Analyte Entry Fixed Maximum Titrant Volume 20 000 mL Potential Range 2000 0 to 2000 0 mV Volume Flow Rate 25 mL 50 0 mL min Signal Averaging 1 Reading Significant Figures XXXXX CALCULATIONS Calculations Sample Calc by Volume Titrant ...

Page 191: ...be vapor saturated minimizing evaporation Place the narrow neck beaker on an analytical balance Zero the balance Place the dosing tip through the neck of the beaker Take care not to immerse it in the liquid during dispensing and not to touch the beaker walls Press Write down the exact weight displaced on the balance after each dose The following information is needed to verify the accuracy of the ...

Page 192: ...he HI762070C 70 C temperature key to the RCA socket temperature sensor input on Analog Board 1 The titrator should display ATC 70 0 0 4 C with no fluctuations or drift This procedure can be repeated on analog board 2 TEMPERATURE MV CHANNEL LOGGING PROCEDURE Connect the shorting cap to the BNC socket on Analog Board 1 Connect the HI762000C 0 C temperature key to the RCA socket temperature sensor in...

Page 193: ...minimizing evaporation Place the narrow neck beaker on an analytical balance Zero the balance Place the dosing tip through the neck of the beaker Take care not to immerse it in the liquid during dispensing and not to touch the beaker walls Press Write down the exact weight displaced on the balance after each dose The following information is needed to verify the accuracy of the dosing system The t...

Page 194: ...l standard weigh ρSTD 8 g mL Temperature C Factor 17 0 1 002290 18 0 1 002467 19 0 1 002654 20 0 1 002853 21 0 1 003061 22 0 1 003282 23 0 1 003512 24 0 1 003752 25 0 1 004002 26 0 1 004261 27 0 1 004531 28 0 1 004809 29 0 1 005097 30 0 1 005395 STIRRING SPEED FAST CHECK PROCEDURE On the main screen select if necessary select the analog board and press Press and use the arrow keys to highlight Sti...

Page 195: ...TITRATION THEORY AUTOMATIC POTENTIOMETRIC TITRATOR HI932 HI931 ...

Page 196: ...2 ...

Page 197: ...7 REDOX TITRATIONS 2 2 8 KARL FISCHER TITRATION 2 3 TITRATIONS ACCORDING TO THE TITRATION SEQUENCE 2 3 1 BACK TITRATIONS 2 3 2 MULTIPLE ENDPOINT TITRATIONS 3 INTRODUCTION TO TITRATION APPARATUS AND TYPICAL TITRATION PROCEDURE 3 1 MANUAL TITRATION 3 2 AUTOMATIC TITRATION 4 TITRATION RESULTS 4 1 ACCURACY 4 2 REPEATABILITY 4 3 SOURCES OF ERROR 4 3 1 SAMPLING ERRORS 4 3 2 ERRORS WITH TITRANT AND STAND...

Page 198: ...4 ...

Page 199: ...reaction ratios A convenient endpoint or inflection point Titrations are highly precise and can provide many advantages over alternative methods Titrations are quickly performed and require relatively simple apparatus and instrumentation 1 2 USES OF TITRATIONS Titrations can be used in many applications including Acid content of plant effluents food e g cheese and wine plating and etching baths pe...

Page 200: ...e and gives current but the reacted species does not In B the reactant is not active but the titrant is In C both the analyte and titrant are active and both give current flow Graph D shows the same situation as B however the current has an opposite sign the titrant is reduced Figure 1 2 1 2 POTENTIOMETRIC TITRATIONS Potentiometric titrations are done by measuring the voltage across the solution u...

Page 201: ...dicator or by one of the reactants or products can be used to monitor the titration In the first titration curve Figure 3 A the absorption of a metal indicator complex is being monitored The absorption is constant while the metal is complexed by the EDTA titrant The metal indicator complex was stripped causing a sharp breakinthetitrationcurve Thepointwhereallthemetaliscomplexedandstrippedfromthein...

Page 202: ... H3 O Ka and pH pKa The color change region is usually 1 pH unit around this point Table 1 contains a list of some aqueous acid base chemical indicators as well as the pH range the pKa and the expected color acid and base form When choosing the proper indicator you should select one that has a pKa as close to the endpoint of the titration When chemical indicators are not suitable a potentiometric ...

Page 203: ... ISE for chloride titrations and a reference electrode Figure 5 shows the titration of 50 mL of 0 1N NaCl with 0 1N AgNO3 The potentiometric signal is from a chloride ISE and is plotted as pCl log Cl Figure 5 2 2 3 COMPLEXOMETRIC TITRATIONS A complex is a species where a central metal ion is covalently bonded to one or more electron donating groups called ligands In a complexometric titration meta...

Page 204: ...t added 2 2 5 NON AQUEOUS SOLVENT ACID BASE TITRATIONS Non aqueous solvents must be used to titrate very weak acids and bases due to Figure 7 the inherent leveling effect water has on all acids and based dissolved in it A wide variety of weak acids and bases can be titrated using non aqueous solvents Mixtures of acids or bases can often be individually analyzed in a single sequential titration TIT...

Page 205: ...lead and zinc salts are titrated using this method The chemical reactions must form an insoluble salt and precipitate out quickly in order to be analyzed by this method When the reaction is not quick a back titration can be used A measured excess of the precipitating reagent titrant is added to force the reaction to occur and then unreacted titrant is then titrated with a standard solution of anot...

Page 206: ...S ACCORDING TO THE TITRATION SEQUENCE 2 3 1 BACK TITRATIONS Back titrations are generally used when a reaction is too slow to be directly accomplished using a direct titration where the reaction goes to completion within a few seconds In a back titration a large excess of a reagent is added to the sample solution helping a slow reaction to go to completion The unreacted excess reagent is then titr...

Page 207: ...ignals the reaction endpoint 5 The concentration of analyte is calculated based on the concentration and volume of titrant required to reach the endpoint 3 2 AUTOMATIC TITRATION Automatic titrators are high precision analytical instruments that deliver the titrant monitor the physical change associated with the titration reaction automatically stop at the endpoint and calculates the concentration ...

Page 208: ...ility or the agreement between replicate determinations is expressed quantitatively as the relative standard deviation RSD 4 3 SOURCES OF ERROR One of the advantages of volumetric analysis is excellent accuracy and precision The sources of error can be grouped into sampling titrant and standards chemical reactions endpoint determination and calculations 4 3 1 SAMPLING ERRORS Selection of a non hom...

Page 209: ...second derivative The inflection point of the titration curve mV vs Volume is normally assumed to be the equivalence point The first derivative is often used to determine the inflection point The maximum value of the first derivative dmV vs dV corresponds to the theoretical equivalence point During a titration it is rare to have a data point exactly at the first derivative maximum the maximum valu...

Page 210: ...ume C sample Sample Concentration g 100mL V titrant Volume of titrant L C titrant Titrant Concentration eq L Ratio Equivalence ratio of analyte titrant mol analyte eq titrant FW analyte Formula Weight of the Analyte g mol V sample Volume of Sample mL 5 2 STANDARDIZE TITRANT Titrant standardization is the second most important calculation in titrations A primary standard is titrated in order to det...

Page 211: ...eq L V sample Volume of Titrant required for the sample L V blank Volume of Titrant required for the blank L Ratio Equivalence ratio of analyte titrant mol analyte eq titrant FW analyte Formula Weight of the Analyte g mol m sample Mass of sample g 5 4 MULTIPLE ENDPOINT TITRATION Some titrations have two or more endpoints each corresponding to the equivalence point for a specific reaction Multiple ...

Page 212: ...ncentration of titrant 2 N V titrant 2 Volume of titrant 2 L Ratio Equivalence ratio of analyte titrant mol analyte eq titrant FW analyte Formula Weight of the analyte g mol V sample Volume of sample mL 6 GLOSSARY Acid A chemical species that can donate one or more protons hydrogen ions Acid Base Titration Stoichiometric neutralization titrations based upon the reaction that occurs between an acid...

Page 213: ... point A fixed value endpoint pH or mV can be used as well The titration will stop at the desired point regardless if the titration is complete Equivalence point The point where the quantity of titrant is stoichiometrically equal to the quantity of analyte Formal The theoretical number of equivalents per liter of the solution It is used in solutions where the exact concentration of a species may b...

Page 214: ...ed to titrate very weak acids and bases to eliminate the leveling effect water has on all acids and bases dissolved in it Normal The concentration of a solution which accounts for any stoichiometric difference between the various species in a solution Oxidation Reduction Potential ORP The measurement describing whether a species wants to donate or accept electrons from other species in a redox rea...

Page 215: ...ation in sample measurements taken by a single person or instrument under the same conditions Spectrophotometric Titration A titration in which the endpoint is marked by a change in the color and or color intensity Stoichiometry The quantitative relationship of the reactants and products in a chemical reaction Titrant The chemical added in a titration that causes the given reaction to occur Titrat...

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Page 218: ...l Park 584 Park East Drive Woonsocket RI 02895 USA www hannainst com Local Office Hanna Instruments Inc Highland Industrial Park 584 Park East Drive Woonsocket RI 02895 USA Phone 800 426 6287 Fax 401 765 7575 e mail tech hannainst com MAN931 Printed in ROMANIA ...

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