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5-16

METHODS

5.5.10

Control Parameters

The user can access and edit the parameters related to the titration.

5.5.10.1 Titration Speed

Choose the desired titration speed for the method. Some samples or reagents may produce
very abrupt endpoints, requiring slower titration speeds in order to avoid over-titration.

Summary of Contents for HI 904

Page 1: ...1 QUICK START GUIDE HI 904 KARL FISCHER COULOMETRIC TITRATOR Revision 1 0 www hannainst com...

Page 2: ...y information for the correct use of the instrument The purpose of this guide is to present a quick overview of setting up and using the instrument For detailed information illustrating the extensive...

Page 3: ...s INTRODUCTION 5 SAFETY MEASURES 6 TITRATOR CONNECTIONS 7 USER INTERFACE 8 HOW TO SELECT YOUR LANGUAGE 9 HOW TO USE THE CONTEXTUAL HELP 9 METHODS 9 BEFORE PERFORMING THE FIRST TITRATION 10 HOW TO PERF...

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

Page 5: ...ntain the constant current between the pins of the electrode The endpoint detection algorithm incorporated in the HI 904 analyzes both the electrode response to individual additions of iodine and the...

Page 6: ...e properly assembled 3 Always wipe up spills and splashes immediately 4 Avoid the following environmental working conditions Severe vibrations Direct sunlight Atmospheric relative humidity above 80 no...

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

Page 8: ...acklit color display The Standby Mode screen is shown below with short explanations The user interface contains several screens In each screen many information fields are present at the same time The...

Page 9: ...xtual help can be accesed at any time and it provides useful information about the current screen METHODS The HI 904 Karl Fischer titrator can store up to 100 methods these include up to 90 standard m...

Page 10: ...ysis we will use the HI 9301EN Moisture in Solvent To select this method Press from the Idle screen Use the and keys to highlight the HI 9301EN Moisture in Solvent method Press After accomplishing the...

Page 11: ...omatic Drift Entry is selected The titrator calculates the rate of atmospheric moisture seeping into the titration beaker for the next minute and displays the result in the lower right corner of the d...

Page 12: ...e Performing a Titration From the main screen press for analyzing a sample You will be prompted to enter the analyte size Add a prepared sample according to a preparation method outlined above Enter t...

Page 13: ...er the mV value remains below the end point potential for the selected stability time When the titration has ended the titrator will display the final concentration of the moisture together with the b...

Page 14: ...sage Printing will be displayed on the screen Press to return to the Data Parameters screen Press again to return to the main screen Saving the data on a USB storage device This feature allows saving...

Page 15: ...d 1 Any text Field 2 Any text Field 3 Any text Titrator Software Version v1 00 Base Board Software Version v3 00 Titrator Serial Number 04132903 Analog Board Serial Number 33121212 Analog Calibration...

Page 16: ...379 4 00 00 42 41 104 0 377 8 00 00 43 42 106 9 376 1 00 00 44 66 140 8 101 0 00 01 09 67 141 2 94 1 00 01 10 68 141 2 91 2 00 01 12 69 141 2 89 9 00 01 13 70 141 2 88 8 00 01 14 71 141 2 88 1 00 01 1...

Page 17: ...1 INSTRUCTION MANUAL HI 904 KARL FISCHER COULOMETRIC TITRATOR Revision 1 00 www hannainst com...

Page 18: ...the instrument This manual will provide you with the necessary information for the correct use of the instrument Hanna Instruments All rights are reserved Reproduction in whole or in part is prohibit...

Page 19: ...3 USER INTERFACE Chapter 4 GENERAL OPTIONS Chapter 5 METHODS Chapter 6 TITRATION Chapter 7 AUXILIARY FUNCTIONS Chapter 8 MAINTENANCE PERIPHERALS Chapter 9 OPTIMIZATION Appendix 1 TECHNICAL SPECIFICATI...

Page 20: ...4...

Page 21: ...rts and drift analysis reports can be printed saved on a USB storage device or transferred to a PC via the USB interface Result history Averaging and statistical data available for sample analysis GLP...

Page 22: ...1 2 INTRODUCTION...

Page 23: ...ar View 2 6 2 3 3 Titrator Left side View 2 6 2 3 4 Titrator Assembly 2 7 2 3 4 1 Connecting the Air Pump 2 7 2 3 4 2 Connecting the Reagent Adapter Holder 2 8 2 3 4 3 Titration Vessel 2 9 2 3 4 3 1 T...

Page 24: ...2 2 SETUP...

Page 25: ...c 5 Pump Locking Screw with Plastic Head 2 pcs 6 Reagent Bottle Assembly 1 pc Bottle Cap Desiccant Desiccant Cartridge Fittings O rings Tubes Silicone and PTFE Tubing 7 Waste Bottle Assembly 1 pc Wast...

Page 26: ...ust be returned in their original packing materials together with the supplied accessories 2 2 Safety Measures The following safety measures must be followed 1 Never connect or disconnect the air pump...

Page 27: ...2 5 SETUP 2 3 Installation 2 3 1 Titrator Top View...

Page 28: ...2 6 SETUP 2 3 2 Titrator Rear View 2 3 3 Titrator Left side View...

Page 29: ...nd or replaced with minimal exposure of the interior of the vessel to ambient moisture from atmospheric humidity Connect the air pump with the following steps see Figure 1 1 Retrieve the air pump cabl...

Page 30: ...tubes It is easily removable for cleaning purposes Install the Reagent Adapter Holder with the following steps see Figure 2 1 Lower the Reagent Adapter Holder base into the right bay then slide it tow...

Page 31: ...h open top screw cap for easy septum replacement A desiccant cartridge containing molecular sieves to dry the ambient air which enters the cell as reagent and sample are added removed from the titrati...

Page 32: ...ttach to the titration vessel A in the dedicated ground glass port Karl Fischer Generator Electrode The Karl Fischer generator electrode D consists of two platinum electrodes anode and cathode on a gl...

Page 33: ...eration if lower drift is not necessary Otherwise place the supplied glass stopper G in the Reagent Exchange Port Sample Port The sample port consists of a silicone rubber septum B secured in place wi...

Page 34: ...tor A Power switch B Power input connector 24 Vdc DC Power jack connector C Generator electrode output 5 pin connector D Detector electrode input BNC socket E External magnetic stirrer 4 pin mini DIN...

Page 35: ...Karl Fischer reagents give off harmful vapors Consult manufacturer s MSDS for safe handling guidelines To assemble the reagent or waste bottle see Figure 6 and follow the next steps Insert a PTFE top...

Page 36: ...r see Figure 7 1 Loosen the compression caps on the Reagent Exchange Adapter so that the o rings uncompress 2 Slide the blue PTFE reagent tube from the reagent bottle assembly through the cap and o ri...

Page 37: ...nction Keys 3 4 3 2 1 2 Option Keys 3 4 3 2 1 3 Arrow Keys 3 5 3 2 1 4 Numeric Keys 3 5 3 2 1 5 Enter Key 3 5 3 2 2 Display 3 5 3 2 3 The Idle Screen 3 6 3 2 4 The Process Screen 3 7 3 3 Menu Navigati...

Page 38: ...3 2 USER INTERFACE...

Page 39: ...rator using the power switch located on the back of the instrument Wait until the titrator finishes the initialization process Press when prompted or wait a few seconds for titrator to start Note All...

Page 40: ...s is pressed the associated function is immediately performed Some of the keys are only active in specific screens Starts or stops titration sequence Turns the stirrer ON and OFF Idle mode only Reserv...

Page 41: ...umeric entries Toggles between positive and negative values Decimal point Initiates entry of exponent for scientific notation 3 2 1 5 Enter Key Both keys perform the same functions Accepts alphanumeri...

Page 42: ...plays the name of the selected method Time and date Displays the current date and time Stirrer information Actual Set stirrer speed is displayed in RPM When stirrer is off the stirrer information is n...

Page 43: ...d time Process stage field Displays the current process Pre titration Drift Analysis Standby Sample Analysis Process status Displays the process status with a descriptive drawing mV reading Displays t...

Page 44: ...ys 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...

Page 45: ...ng 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 con...

Page 46: ...3 10 USER INTERFACE...

Page 47: ...4 4 Stirrer 4 5 4 5 Language 4 6 4 6 Reagent Exchange Reminder 4 6 4 7 Save Files to USB Storage Device 4 7 4 8 Restore Files from USB Storage Device 4 8 4 9 USB Link with PC 4 9 4 10 Calibration Che...

Page 48: ...4 2 GENERAL OPTIONS...

Page 49: ...mode In Pre titration Drift Analysis Standby or Titration process the General Options can be accessed by pressing the Home key on a PS 2 keyboard The available menus are described below 4 1 Date and T...

Page 50: ...om 0 to 7 A color palette is displayed in the center of the screen allowing an easy selection of the appropriate backlight intensity The backlight saver option protects the display during standby peri...

Page 51: ...hen a critical error occurs during titration 4 4 Stirrer This screen allows the user to select the internal magnetic stirrer an external magnetic stirrer or a user controlled stirrer uncontrolled by t...

Page 52: ...r have been titrated Coulometric Karl Fischer reagents also have a tendency to produce precipitates and foul smelling sulfurous compounds This is particularly problematic when using a diaphragm genera...

Page 53: ...s The number of files and each file name on the titrator will be displayed Use the and keys to scroll through the list The option keys allow the following operations Returns to the General Options scr...

Page 54: ...and keys to scroll through the list The number of files and the name of each file found on the USB storage device is displayed on the screen The option keys allow the following operations Returns to...

Page 55: ...r is not connected to the HI 900 PC Application Active The titrator is connected to the HI 900 PC Application Ready The titrator is ready for commands Transmit It shows the progress of the current tra...

Page 56: ...Set the multimeter to A mode If necessary switch the calibration key to A mode by pressing the red button Connect the calibration key banana plugs to the multimeter mA input Check for the multimeter i...

Page 57: ...ction with the balance is working properly by pressing the key 4 12 Printer mode This screen allows the user to select the printing mode ANSI default ASCII and Text mode ANSI mode Use this mode when y...

Page 58: ...be careful This will also delete all the user created methods reports and restore all manufacturer settings such as titrator configuration standard method parameters etc 4 14 Update Software This scr...

Page 59: ...6 5 5 Method Options 5 7 5 5 1 Naming the User Method 5 7 5 5 2 Method Revision 5 8 5 5 3 Method Type 5 8 5 5 4 Pre Analysis Stir Time 5 9 5 5 5 Stirring Speed 5 9 5 5 6 Stirbar Type 5 10 5 5 7 Drift...

Page 60: ...rent 5 18 5 5 10 5 End Point Value 5 18 5 5 10 6 Generator Current Mode 5 19 5 5 10 7 Signal Averaging 5 19 5 5 11 Termination Parameters 5 20 5 5 11 1 Maximum Duration 5 20 5 5 11 2 Maximum Titrated...

Page 61: ...ting the titrator to a PC using the HI 900 PC application or a USB storage device 5 1 Selecting Methods To select a method press the key when available A list of available methods will be displayed In...

Page 62: ...n the storage device will be displayed Press the or key to upgrade the titrator with the standard methods Press to return to General Options screen Note See section 4 8 Restore Files from USB Storage...

Page 63: ...ifying 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...

Page 64: ...hod press when available Highlight the user method that you want to delete and press A screen will appear in order to confirm the deletion Press again to confirm or press to cancel the operation 5 4 V...

Page 65: ...e Method to keep the changes 5 5 Method Options 5 5 1 Naming the User Method This option allows you to enter a name for the new method up to 24 characters Use the arrow keys to navigate through the ch...

Page 66: ...presenting the current method revision The revision string format should be X Y where X and Y are numerical digits 5 5 3 Method Type Method type is a parameter listed in each method In order to conduc...

Page 67: ...ir time can be set between 5 and 1000 seconds After the sample is added to the reaction vessel the titrator will stir for the set period of time before any iodine is generated bromine is consumed 5 5...

Page 68: ...is used during the titration process Automatic the drift rate will be calculated automatically after the Pre titration of the solvent User the drift is set to a fixed value entered by the user The us...

Page 69: ...1 METHODS 5 5 8 Reagent The user can enter a name for the reagent up to 15 characters Use the arrow keys to navigate through the character table press to add the highlighted character to the reagent n...

Page 70: ...for the preparation of insoluble samples that require a water extraction Using the proper solvents the sample is broken down into a fine suspension from which the water is extracted and released into...

Page 71: ...to navigate through the character table Press to add the highlighted character to the sample name 5 5 9 3 Sample Type Normal Determination only This option allows the user to select the type of the s...

Page 72: ...tion is started the user is asked again to enter the sample size The sample size mass or volume can be automatically acquired from the balance when the balance feature is enabled see Section 4 11 Setu...

Page 73: ...ter content but before adding sample to the solvent 5 5 9 7 External Solvent Conc External Dissolution Extraction determination modes only Enter the concentration of water in the solvent 5 5 9 8 Extra...

Page 74: ...cess and edit the parameters related to the titration 5 5 10 1 Titration Speed Choose the desired titration speed for the method Some samples or reagents may produce very abrupt endpoints requiring sl...

Page 75: ...vert to Standby mode after a titration is completed See also the Standby Duration option 5 5 10 3 Standby Duration The user can enter the period of time which the cell is kept dry and ready for subseq...

Page 76: ...arization current from the predefined list Note Higher polarization currents will speed the contamination of the electrode and potentially degrade samples 5 5 10 5 End Point Value This option defines...

Page 77: ...ce enough current depending on the Generator Current Mode an error message will be displayed and the titration will be stopped 5 5 10 7 Signal Averaging This option enables averaging of the mV reading...

Page 78: ...allowed to run Once this point is reached the titration will be terminated even if the end point is not reached The time can be set from 10 to 3600 seconds 5 5 11 Termination Parameters This screen al...

Page 79: ...al drift is less than the predefined absolute drift value Relative Drift The titration is terminated when the actual drift is less than the sum between the initial drift and the predefined relative dr...

Page 80: ...e dedicated socket or if the printer is offline an error message will appear on the display see Section 8 5 3 Connecting a Printer for information about connecting a printer to the titrator 5 5 11 4 E...

Page 81: ...reagent Consult a standard method for preparation instructions 3 Connect the Bromine Index reagent bottle to the titrator and fill the vessel according to Section 2 of the manual 4 Set a method to Br...

Page 82: ...5 24 METHODS...

Page 83: ...6 1 TITRATION Chapter 6 Contents 6 TITRATION 6 3 6 1 Idle 6 3 6 2 Pre titration 6 3 6 3 Drift Analysis 6 4 6 4 Standby 6 5 6 5 Sample Analysis 6 6...

Page 84: ...6 2 TITRATION...

Page 85: ...itration vessel between the min and max marks for best reproducibility The following intermediary stages are performed automatically before starting the analysis Reagent pre titration Drift analysis A...

Page 86: ...round drift rate or the drift rate The drift rate is determined by keeping track of the amount of water that has been titrated to maintain the dryness of the reagent over the course of a minute The ra...

Page 87: ...oard only by pressing Home After an initial titrator setup and prior to the first titration or standardization the drift rate should be allowed to settle in Standby mode for 45 min This ensures that t...

Page 88: ...Standby mode by pressing in order to wait until the drift is stabilized at a higher value Entering estimated concentration The user has the option to enter the estimated concentration The optimal samp...

Page 89: ...lace the full syringe with needle on an analytical balance Tare the balance back weighing technique 7 Insert the needle through the septum in the sample port Push the syringe through the septum until...

Page 90: ...must make sure that the balance and the titrator are properly configured and the balance feature is enabled see Section 4 11 Setup Balance Interface Procedure 1 Place the syringe containing the sample...

Page 91: ...le size is automatically updated Now the analysis can be started Start Analysis Press to begin analysis Suspend Titration While the titration is in progress you can temporarily stop it by pressing The...

Page 92: ...p the titration manually and return to Idle mode Press to stop the titration and return to Standby mode When the end point is reached the titration is finished and the following screen is displayed Th...

Page 93: ...istory Averaging and Statistical Data can be viewed Use the and keys to scroll the results list Use to choose the results that will be used for averaging Note When there are no results selected dashes...

Page 94: ...6 12 TITRATION...

Page 95: ...7 3 7 1 Air Pump 7 3 7 1 1 Filling the Vessel 7 3 7 1 2 Emptying the Vessel 7 3 7 2 Stirrer 7 4 7 3 Results 7 4 7 3 1 Review Last Titration Report 7 5 7 3 2 Review Available Reports 7 5 7 3 3 GLP Data...

Page 96: ...7 2 AUXILIARY FUNCTIONS...

Page 97: ...ify that the bottle top assemblies are properly assembled tightly sealed and that the liquid handling tubing reaches the bottom of the reagent bottle 4 When the level of reagent inside the titration c...

Page 98: ...to the stirrer are not available The stirrer can be turned on and off by pressing while in Idle mode During the titration process the stirrer cannot be turned off The stirring speed is set within the...

Page 99: ...access the following options 7 3 1 Review Last Titration Report The last titration report can be reviewed The information seen in the report is based on the selections made in the Setup Titration Repo...

Page 100: ...reviewed and printed The report contains only the information selected in the Setup Titration Report screens during report generation The following option keys are available Review the titration graph...

Page 101: ...titrator configuration data Titrator Serial Number The serial number of the titrator base board Analog Board Serial Number The serial number of the titrator analog board Titrator Software Version The...

Page 102: ...7 8 AUXILIARY FUNCTIONS 7 3 5 Setup Titration Report Customize a unique report to record the titration results An asterisk means that it will be included in the titration report...

Page 103: ...ance 8 3 8 2 Detector Electrode Maintenance 8 3 8 3 Reagent Adapter Holder Maintenance 8 4 8 4 Reagent Exchange Adapter Maintenance 8 4 8 5 Peripherals 8 5 8 5 1 Connecting an External Display 8 5 8 5...

Page 104: ...8 2 MAINTENANCE PERIPHERALS...

Page 105: ...ragm to clear it of possible contaminants For a more thorough cleaning allow 1 or 2 more aliquots of dry methanol to diffuse through the diaphragm 5 Wipe joint grease off of the ground glass joints wi...

Page 106: ...ge Avoid using brushes abrasives to clean the pins Pins can easily bend which will cause permanent errors in mV readings 8 3 Reagent Adapter Holder Maintenance The glass tube of the reagent adapter ho...

Page 107: ...eripherals Warning Connection disconnection of POWER CORD PUMP ASSEMBLY EXTERNAL PC DISPLAY PRINTER RS232 INTERFACE or EXPANSION DEVICE must be done only when titrator and external devices are turned...

Page 108: ...INTENANCE PERIPHERALS 8 5 2 Connecting an External PC Keyboard This connection allows you to use an external PS 2 PC Keyboard in addition to titrator s keypad Connect an external PC Keyboard PS 2 conn...

Page 109: ...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 F...

Page 110: ...inters can be connected to the parallel port of the titrator using a standard DB 25 cable Warning The titrator and the external printer must both be OFF before they are connected Connect the external...

Page 111: ...able to the USB port on the rear panel of the titrator Connect the cable to the USB port on the PC Select the USB Link with PC screen on the titrator by following the path General Options USB Link wit...

Page 112: ...8 10 MAINTENANCE PERIPHERALS...

Page 113: ...mination Parameters 9 5 9 1 2 1 Stability Time 9 5 9 1 2 2 Drift Stop Termination Criteria 9 5 9 1 2 2 1 Relative Drift Stop 9 5 9 1 2 2 2 Absolute Drift Stop 9 6 9 1 3 Method Options 9 6 9 1 3 1 Pre...

Page 114: ...ple Preparation Techniques 9 9 9 2 5 1 Dilutions 9 9 9 2 5 2 External Dissolution 9 9 9 2 5 3 External Extractions 9 9 9 2 5 4 Homogenization 9 1 0 9 2 5 5 Heating 9 1 0 9 3 Karl Fischer Reagent Syste...

Page 115: ...pins of the electrode At the endpoint of the titration the amount of iodine added is equal to the amount of water from the sample When an excess of iodine has been generated the excess iodine is easi...

Page 116: ...f titrant beyond the endpoint and provides enhanced data density in the vicinity of the endpoint resulting in accurate endpoint determination and faster titrations The minimum and maximum dose volume...

Page 117: ...e distinguished by the way in which the drift rate thresholds are specified 9 1 2 2 1 Relative Drift Stop The relative drift stop termination parameter should be the first choice termination criteria...

Page 118: ...ring Speed The HI 904 s stirring speed can be set between 200 and 2000 RPM with 100 RPM resolution The stirring system is equipped with an optical feedback mechanism to ensure that the stirring motor...

Page 119: ...ample Ideally the sample size would be scaled to always be in this range but it becomes impractical to add the large sample sizes that would be required for concentrations of 500 ppm and lower Attempt...

Page 120: ...o the wall of the titration vessel electrode or dispensing tip 9 Draw a small amount of air from inside the cell into the syringe to ensure that no sample drops remain on the tip of the needle 10 Remo...

Page 121: ...for sample dilutions If the sample contains fats or oils then a mixture of methanol and chloroform can be used to promote solubility of the sample The following outlines a generic dilution procedure...

Page 122: ...be evenly distributed throughout a collected sample by the use of high speed high shear mixers called homogenizers In mixed phase oil and water non aqueous samples water tends to migrate to the surfa...

Page 123: ...0 GMP GLP and FDA guidelines for water determination Water standards are available commercially in single use sealed ampoules Concentration values are typically 0 1 1 0 and 10 0 mg g and are certified...

Page 124: ...9 12 METHODS OPTIMIZATION...

Page 125: ...A3 2 APPENDIX 3...

Page 126: ...A3 6 APPENDIX 3 MAN HI904 09 13...

Page 127: ...A1 1 APPENDIX 1 Appendix 1 Contents A1 TECHNICAL SPECIFICATIONS A1 3...

Page 128: ...A1 2 APPENDIX 1...

Page 129: ...ating Volume 100 200 mL Septum Silicone rubber Septum Cap Thread GL 18 Reagent Port Standard Taper 19 Detector Electrode Type Dual platinum pin polarization electrode Electrical Connection BNC Glass C...

Page 130: ...nitor Instrument status and titrations can be viewed on a larger screen using any VGA compatible external monitor Keyboard Alphanumeric text can be entered using an optional PS 2 keyboard Graphic Disp...

Page 131: ...1 APPENDIX 2 Appendix 2 Recommended Reagents A2 RECOMMENDED REAGENTS A2 3 A2 1 Reagents for Generators with Diaphragm A2 3 A2 2 Reagents for Generators without Diaphragm A2 3 A2 3 Water Standards A2...

Page 132: ...A2 2 APPENDIX 2...

Page 133: ...rocarbons Oils 34843 Coulomat AG H anolyte 34840 Coulomat CG catholyte Hydrocarbons Oils 34820 Coulomat AK anolyte 34821 Coulomat CG K catholyte Ketones Aldehydes A2 2 Reagents for Generators without...

Page 134: ...A2 4 APPENDIX 2...

Page 135: ...A3 1 APPENDIX 3 Appendix 3 Accessories A3 TITRATOR COMPONENTS A3 3...

Page 136: ...A3 2 APPENDIX 3...

Page 137: ...or Electrode HI 900511 Generator Electrode with Diaphragm HI 900512 Generator Electrode without Diaphragm HI 900180 Air Pump HI 900181 Reagent Adapter Holder Assembly A3 TITRATOR COMPONENTS HI 900182...

Page 138: ...te Bottles HI 900535 2 x Tubing for Reagent Waste Handling HI 900536 2 x Tubing for Air Pump HI 900566 Open top GL18 Cap HI 900563 Glass Stopper Standard Taper 19 HI 900564 Desiccant Cartridge for Gen...

Page 139: ...A3 5 APPENDIX 3 HI 900804 Manual English for HI 904 HI 900900U PC Application on USB Flash Drive HI 920013 USB Cable HI 900567 Septum Kit 5 pcs HI 900543 Glass Joint Grease HI 900931 Generator Cable...

Page 140: ...A3 6 APPENDIX 3 MAN HI904 09 13...

Page 141: ...1 GENERAL APPLICATIONS BROCHURE HI 904 KARL FISCHER COULOMETRIC TITRATOR www hannainst com...

Page 142: ......

Page 143: ...1 mL into the titration vessel through the septum using the needle Pay attention not to get any standard on the electrode or beaker walls If necessary swirl the titration vessel by hand Clear the need...

Page 144: ......

Page 145: ...ple size Dispense 0 8000 g to 1 0000 g of solvent into the titration vessel through the septum using the needle Pay attention not to get any sample on the electrode or beaker walls If necessary swirl...

Page 146: ......

Page 147: ...art Stop to pre titrate the reagent Fill the syringe and needle with the sample Weigh the syringe needle and sample Press Start Analysis You will be prompted to enter the sample size Enter the Estimat...

Page 148: ...Applications r 1 0 Results Titration Report Method Name BrIndex of Aromatics Time Date 12 00 Jan 01 2013 Sample Size 0 4978 g Bromine Consumed 1 609 mg Result 323 33 mg 100g Titration Duration 4 36 mm...

Page 149: ...1 TITRATION THEORY TITRATION THEORY Principles HI 904 KARL FISCHER COULUMETRIC TITRATOR Revision 1 0 www hannainst com...

Page 150: ...2 TITRATION THEORY...

Page 151: ...3 2 Generator Electrode without Diaphragm 11 2 2 1 4 Visual Indication of Karl Fisher Titrations 12 2 2 1 5 Electrometric Indication of Karl Fisher Titrations 12 2 2 2 Acid Base Titrations 13 2 2 3 Ar...

Page 152: ...ontent as mass subtracting Background Drift Rate 23 5 1 5 Calculation of water content in External Dissolution Samples 24 5 1 6 Calculation of water content in External Extraction Samples 24 5 1 7 Cal...

Page 153: ...or by some other physical measurement Titrations cannot be used to determine the quantity of all analytes The chemical reaction between the titrant and analyte must fulfill four requirements The reac...

Page 154: ...osts and easy training Suitability to measure major components of a mixture or product Automation can reduce time and labor spent on each analysis Some disadvantages of titrations are Time it takes to...

Page 155: ...he change in the electroactivity of the solution Many metal ions can be amperometrically titrated using a precipitation complexation or redox reaction Some metal ions and species that can be determine...

Page 156: ...hat change color during the course of the titration are available for many titrations More accurate data on the titration curve can be obtained if the light absorption is monitored instrumentally usin...

Page 157: ...nation by Karl Fischer titration is based on the reaction described by Bunsen in 1853 in which sulfur dioxide is oxidized by iodine in the presence of water I2 SO2 2 H2O g 2 HI H2SO4 In Karl Fischer s...

Page 158: ...em or by the solvent two component system One component reagent systems can utilize a custom solvent or solvent mixture since all of the Karl Fischer reaction components are in the titrant However one...

Page 159: ...cross the diaphragm during drift analysis and sample analysis and will add to the apparent drift rate The second disadvantage is the risk of diaphragm blockage or contamination Substances in the sampl...

Page 160: ...n are the two types of electrometric detection methods commonly used for indication of Karl Fischer titrations Both methods use either a double platinum pin or a double platinum ring electrode to dete...

Page 161: ...reproducible titrations Second the accuracy of electrometrically indicated titrations are not affected by the over titration because the slight excess of iodine has been accounted for during the stan...

Page 162: ...These titrations are commonly used to titrate and determine the concentration of bromide chloride cyanide iodide and sulfide Argentometric titrations can be done with Mohr s indicator when all of the...

Page 163: ...ng an indicator electrode that responds to the metal ion see Figure 5 2 2 5 Ion Selective Titrations The most popular ion selective titration is an acid base titration The hydrogen ion concentration i...

Page 164: ...rable compounds The endpoint for non aqueous titrations are usually determined potentiometrically using a pH glass electrode a modified calomel or double junction reference electrode with a low flow r...

Page 165: ...d The difference in the total volume of the first reagent added and amount determined from the second titration is the quantity of reagent required to complete the first reaction 2 3 2 Multiple End Po...

Page 166: ...18 TITRATION THEORY A B Figure 8 Potential glass electrode mV C...

Page 167: ...known concentration A visual or instrumental indicator for detecting the completion of the reaction A typical manual titration consists of the following steps 1 A volumetric pipette is typically used...

Page 168: ...very low gear backlash in the burette pump minimal piston seal flexing precision ground inner diameter of the glass syringe a low dead volume valve minimal evaporation permeation and chemically resis...

Page 169: ...s or non representative sample Sample changed or was contaminated during collection storage or transfers Poor technique when transferring sample to beaker or flask Errors in the balance calibrate and...

Page 170: ...irst derivative and second derivative The inflection point of a potentiometric curve mV vs Volume is normally assumed to be the equivalence point The first derivative is often used to determine the in...

Page 171: ...Titrant mL Titer Titrant Titer mg mL V sample Volume of Sample mL d sample Density of Sample g mL 5 1 3 Calculation of water content as volume from samples measured by volume C sample Concentration of...

Page 172: ...s Samples The water content of gases is normally reported in units of g L or mg L C sample Concentration of Sample mg L V titrant Volume of Titrant mL Titer Titrant Titer mg mL Flow Rate Sample Flow R...

Page 173: ...tration g 100g V titrant Volume of titrant C titrant Titrant Concentration eq L Ratio Equivalence ratio of analyte titrant mol analyte eq titrant FW analyte Formula Weight of the Analyte g mol m sampl...

Page 174: ...ution matrix The basic titration equation can be used for a blank titration with the single modification that the volume of titrant used in the blank titration should be subtracted from the regular ti...

Page 175: ...ht of Sample mL 5 2 5 Back Titration The equation used in back titration calculations is also similar to the equation for a blank titration Instead of subtracting the initial amount of titrant needed...

Page 176: ...sults Back Titration A type of titration where an excess amount of titrant is added to a sample forcing a sluggish reaction to go to completion The excess reagent is then back titrated with a second t...

Page 177: ...y used in manual titrations Chemical indicators have been replaced with electrometric indicators which are used with automatic titrators Inflection Point The point on a titration curve were the second...

Page 178: ...s determined by monitoring the voltage of the solution using an electrode Precipitation Titration A titration in which the analyte reacts with the titrant to form an insoluble compound The end point i...

Page 179: ...lumetric procedure used in analytical chemistry to determine the concentration of an analyte in solution The concentration of the analyte is determined by slowly adding a titrant to the solution As th...

Page 180: ...32 TITRATION THEORY Titr THEORY 904 07 13...

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