Hanna Instruments HI 903 Quick Start Manual
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Hanna Instruments HI 903 Quick Start Manual

Karl fischer volumetric titrator
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QUICK START GUIDE
HI 903
KARL FISCHER
VOLUMETRIC TITRATOR
Revision 1.0
1

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  • Page 1 QUICK START GUIDE HI 903 KARL FISCHER VOLUMETRIC TITRATOR Revision 1.0...
  • Page 2 Dear customer, Congratulations on choosing a Hanna Instruments Product. This guide has been written for the HI 903 Karl Fischer Volumetric Titrator. Please read this Quick Start Guide carefully before using the instrument. This guide will provide you with the necessary information for the correct use of the instrument.
  • Page 3 QUICK START GUIDE Contents INTRODUCTION ......................3 SAFETY MEASURES.....................4 TITRATOR CONNECTIONS ..................5 USER INTERFACE ......................6 HOW TO SELECT YOUR LANGUAGE ................7 HOW TO USE THE CONTEXTUAL HELP ...............7 METHODS ........................7 BEFORE PERFORMING THE FIRST TITRATION............8 HOW TO PERFORM THE FIRST TITRATION ..............9...
  • Page 4 QUICK START GUIDE...

  • Page 5: Introduction

    The HI 903 finds a titration endpoint using a polarized electrode and an advanced detection algorithm. A constant flow of current is maintained between the two platinum pins of the titrator’s electrode.

  • Page 6: Safety Measures

    QUICK START GUIDE SAFETY MEASURES The following safety measures must be followed: 1. Always ensure that the power supply cable is connected to a grounded main power plug. 2. Never connect or disconnect the pump assemblies with the titrator turned on. 3.

  • Page 7: Titrator Connections

    QUICK START GUIDE TITRATOR CONNECTIONS Front View Rear View...

  • Page 8: User Interface

    QUICK START GUIDE USER INTERFACE Keypad The titrators have their own keypad with 29 keys grouped in four categories, as follows: Display The titrators have a 5.7” graphical backlit color display. The Standby Mode screen is shown below with short explanations. The user interface contains several screens.

  • Page 9: How To Select Your Language

    . The contextual help can be accesed at any time and it provides useful information about the current screen. METHODS The HI 903 Karl Fischer titrator can store up to 100 methods: these include up to 90 stan- dard methods. Standard Methods Each titrator is supplied with a customized package of standard methods.
  • Page 10 QUICK START GUIDE BEFORE PERFORMING THE FIRST TITRATION Setup the Titrator • Make sure that all of the titrator assemblies are properly installed (see Instruction Manual, Setup section). • Make sure that the beaker system is properly sealed against atmospheric moisture (the fittings and tubes are correctly mounted).

  • Page 11: How To Perform The First Titration

    QUICK START GUIDE HOW TO PERFORM THE FIRST TITRATION Method Selection For this analysis we will use the HI8301EN Solvent with 5mg/ml 1-component Titrant standard method . To select this method: from the Idle screen. Use the • Press keys to highlight the HI8301EN Solvent with 5mg/ml 1-component Titrant method.
  • Page 12 QUICK START GUIDE • Highlight the Setup Titration Report option and press • Mark the fields to be included with the “*” symbol using the keys and press to toggle the selection. • Press and then press to return to the main screen. Fill Titration Beaker with Solvent The titration beaker must be filled with 1-component up to the MIN marker (about 50 mL of solvent):...
  • Page 13 QUICK START GUIDE ible results. Solid Samples: • Solid samples with larger pieces may need to be pulverized or ground in an analyti- cal mill. These samples can be added with a weighing boat by removing the sample port plug. •...
  • Page 14 QUICK START GUIDE Understanding the Displayed Information During a titration, the following screen is displayed: Viewing Graph During Titration Press to display the real time titration graph. The curve displayed is a plot of Electrode Potential vs. Titrant Volume. A dashed horizontal line represents the user selected end point potential. Titration Termination The titration is terminated when the conditions of the Termination Criteria have been met.
  • Page 15 QUICK START GUIDE Review Last Titration Report option and press • The Review Result screen will be displayed. • Use the keys to display information related to the last titration per- formed. See titration report on page 15. Printing the titration report Connect a DOS / Windows compatible printer directly to the DB 25 connector (parallel port) located on the back of the titrator.
  • Page 16 HI903 - Titration Report Method Name: Moisture in Oil Time & Date: 12:00 Jan 01, 2011 Titration ID: KF_00003 Company Name: Hanna Instruments Operator Name: KF Technician Electrode Name: Probe 1 F i e l d text Field 2: Any text...
  • Page 17 QUICK START GUIDE Standby Duration: 720 minutes Imposed Current: 20 uA Minimum Dose: 0.5000 uL Maximum Dose: 30.0000 uL Timed Increment: 1 second End Point Value: 180.0 mV Signal Averaging: 3 Readings Flow Rate: 10.0 mL/min T e r m i n a t i o n P a r a m e t e r s : Maximum Duration: 3600 sec...
  • Page 18 QUICK START GUIDE...
  • Page 19 INSTRUCTION MANUAL HI 903 KARL FISCHER VOLUMETRIC TITRATOR Revision 1.00...
  • Page 20 © 2010 Hanna Instruments All rights are reserved. Reproduction in whole or in part is prohibited without the written consent of the copyright owner, Hanna Instruments Inc., 584 Park East Drive, Woonsocket, Rhode Island 02895, USA.
  • Page 21 TABLE OF CONTENTS Chapter 1. INTRODUCTION Chapter 2. SETUP Chapter 3. USER INTERFACE Chapter 4. GENERAL OPTIONS Chapter 5. METHODS Chapter 6. TITRATION Chapter 7. AUXILIARY FUNCTIONS Chapter 8. MAINTENANCE, PERIPHERALS Chapter 9. OPTIMIZATION Appendix 1. TECHNICAL SPECIFICATIONS Appendix 2. RECOMMENDED REAGENTS Appendix 3.

  • Page 23: Introduction

    INTRODUCTION INTRODUCTION The HI 903 is an automatic volumetric Karl Fischer titrator with high accuracy, great flexibility and repeatability. The titrator is designed to perform titrations for a variety of sample types. The main attributes of this titrator are: Flexibility Support up to 100 titration methods (standard and user defined).
  • Page 24 INTRODUCTION...

  • Page 25: Table Of Contents

    SETUP Chapter 2. Contents SETUP ....................2 - 3 Unpacking ..................... 2 - 3 Safety Measures ..................2 - 4 Installation ................... 2 - 5 2.3.1 Titrator Top View ..................2 - 5 2.3.2 Titrator Rear View ..................2 - 6 2.3.3 Titrator Left-side View .................

  • Page 26: Setup

    SETUP...

  • Page 27: Unpacking

    SETUP SETUP Unpacking The titrator and the accessories are shipped in a single box containing: ITEM QUANTITY Titrator ..............1 pcs. Dosing Pump Assembly ........... 1 pcs. Burette Assembly ............. 1 pcs. • Burette (with 5 mL syringe) • Aspiration Tube with Fittings and Protection Tube •...

  • Page 28: Safety Measures

    SETUP 10 Waste Bottle Assembly ..........1 pcs. • Bottle Cap • Desiccant • Desiccant Cartridge • Fittings, O-rings • Tubes (Silicon and Teflon Tubing) 11 Calibration Key ............1 pcs. 12 Power Cable ............1 pcs. 13 USB Cable ............... 1 pcs. 14 Instruction Manual Binder .........

  • Page 29: Installation

    SETUP 6. Avoid the following environmental working conditions: • Severe vibrations • Direct sunlight • Atmospheric relative humidity above 95% non-condensing • Environment temperatures below 10°C and above 40°C • Explosion hazards 7. Have the titrator serviced only by qualified service personnel. Installation 2.3.1 Titrator Top View...

  • Page 30: Titrator Rear View

    SETUP 2.3.2 Titrator Rear View 2.3.3 Titrator Left-side View...

  • Page 31: Titrator Assembly

    SETUP 2.3.4 Titrator Assembly Note: Assembly operations must be completed before connecting the titrator to the power supply! 2.3.4.1 Connecting the Pumps Dosing Pump: The dosing pump is driven by a stepper motor, which provides 40,000 steps for a single burette volume.
  • Page 32 SETUP Connect the air pump with the following steps (see Figure 2.): (1) Retrieve the air pump cable (PUMP 2) from inside the right bay. Connect the cable to the air pump as shown in Figure 2. The air pump connector is located on the left side of the motor.

  • Page 33: Attaching The Burette

    SETUP 2.3.4.2 Attaching the Burette The 5 mL glass syringe features a highly precise inner diameter, which has been individually verified to produce consistent titrant dosage according to standard ISO 8655. All of the non- glass, wetted syringe and valve components, including the shoulders and plunger cap, are constructed from PTFE to ensure resistance to both degradation due to Karl Fisher titrant and water vapor permeability.

  • Page 34: Attaching The Beaker And Dispensing Tip

    The titration reaction takes place in a closed, conical, glass beaker, sometimes called a titration vessel, reaction vessel, titration cell or reaction cell. The primary design features of the HI 903 titration vessel include the following: • Durability, easy to use, clean and maintain.

  • Page 35: Beaker Top

    SETUP • Place beaker ring (C) onto beaker support with the notches on top (see Figure 6). • Insert the glass beaker (B) into the beaker ring (C). • Add the stir bar to the glass beaker (B). • Carefully place the beaker top onto the beaker (B). Secure in place by pushing the beaker top through the beaker ring (C) with the 4 notches of the beaker ring aligned with the 4 steel pins of the beaker top (A).
  • Page 36 The Karl Fischer electrode consists of two parallel, platinum pins sealed into a 10mm diam- eter glass body. Two steel pins connect the platinum elements to a standard BNC connector, which allows for easy attachment to the HI 903. Attach to the beaker top as follows: •...

  • Page 37: Electrical Connections

    SETUP 2.3.4.4 Electrical Connections • Connect the KF electrode to the BNC connector (C). • Connect the power supply cable to the power supply connector (B). Figure 8 Function Type of Connector Power switch Power supply (115/230 VAC, 50-60 Hz) IEC Power line connector Check on titrator rear panel (K) KF probe...

  • Page 38: Titrant, Solvent, Waste Bottle Assembly

    SETUP 2.3.5 Titrant, Solvent, Waste Bottle Assembly The bottle top assemblies are equipped with desiccant cartridges containing indicating silica gel which ensures that the air passing through the solvent handling system has been dried. The desiccant has a limited capacity to absorb moisture and is typically exhausted after 2 to 4 weeks.

  • Page 39: Solvent / Waste Bottle Assembly

    SETUP (HI 900531) 2.3.5.2 Solvent / Waste Bottle Assembly Caution: Most Karl Fischer solvents give off harmful vapors. Consult manufacturer’s MSDS for safe handling guidelines. To assemble the solvent or waste bottle, see Figure 10 and follow the next steps: •...
  • Page 40 SETUP 2-16...
  • Page 41 USER INTERFACE Chapter 3. Contents USER INTERFACE .................. 3 - 3 Start Up ....................3 - 3 Description .................... 3 - 4 3.2.1 Keypad ....................3 - 4 3.2.1.1 Function Keys ..................3 - 4 3.2.1.2 Option Keys ..................3 - 4 3.2.1.3 Arrow Keys ..................

  • Page 42: User Interface

    USER INTERFACE...

  • Page 43: Start Up

    USER INTERFACE USER INTERFACE Start Up Once the instrument is assembled and installed, follow the steps below to start the titrator: • Connect the instrument to an outlet equipped with a ground wire. Make sure that the voltage of the main power matches that specified by the titrator. •...

  • Page 44: Description

    USER INTERFACE Description Description Description Description Description This chapter describes the basic principles of navigation through the user interface, selecting fields and entering values from the keypad. 3.2.1 Keypad The titrator’s keypad is grouped into five categories, as follows: 3.2.1.1 Function Keys If one of these keys is pressed, the associated function is immediately performed.

  • Page 45: Arrow Keys

    USER INTERFACE 3.2.1.3 Arrow Keys These keys have the following functions: • Move the on-screen cursor. • Increase and decrease the stirrer speed and other settings. • In the alphanumeric screen, to select a character. • To navigate through menu options. 3.2.1.4 Numeric Keys Keys...

  • Page 46: The Idle Screen

    USER INTERFACE 3.2.3 The Idle Screen After start up and initialization, the first screen displayed is the Idle Screen . Idle Screen fields: Method name: Displays 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.

  • Page 47: The Process Screen

    USER INTERFACE 3.2.4 The Process Screen When the user presses while in Idle Screen , all titration related processes are started. The titrator displays the Process Screen . Process Screen fields: Method name: Displays the name of the selected method. Time and date: Displays the current date and time Process stage field:...

  • Page 48: Menu Navigation

    USER INTERFACE 3.3 Menu navigation 3.3.1 Selecting an Option To select an option, simply press the option key below the virtual key. For example, to access the Method Op- tions screen press the option key below it. 3.3.2 Selecting a Menu Item To select an item from the menu screen use the arrow keys to move the cursor.

  • Page 49: Saving Modifications

    USER INTERFACE 3.3.4 Saving Modifications The Saving Method screen allows the user to save the modifications. To exit from 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.
  • Page 51 GENERAL OPTIONS Chapter 4. Contents GENERAL OPTIONS ................4 - 3 Date and Time Setting ................ 4 - 3 Display Settings ................... 4 - 4 Beeper ....................4 - 5 Stirrer....................4 - 5 Language ..................... 4 - 6 Estimated Cell Volume ................4 - 6 Titrant Database .................

  • Page 52: General Options

    GENERAL OPTIONS...

  • Page 53: Date And Time Setting

    GENERAL OPTIONS GENERAL OPTIONS The General Options screen gives access to options that are not directly related to the titration process. To access this screen, press from the main screen while in idle mode. In Pre- titration, Drift Analysis, Standby or Titration process, the General Options can be accessed by pressing the <<Home>>...

  • Page 54: Display Settings

    GENERAL OPTIONS Display Settings This screen allows the user to customize the viewing features of the display. Option Keys: Increases the backlight saver time interval Decreases the backlight saver time interval The backlight intensity can be adjusted using the keys. There are 8 levels of backlight intensity, ranging from 0 to 7.

  • Page 55: Beeper

    GENERAL OPTIONS Beeper This screen allows the user to turn the Beeper On ( Enable ) or Off ( Disable ). The beeper will sound after a titration is completed, when an invalid key is pressed or when a critical error occurs during titration. Stirrer This screen allows the user to select the internal magnetic stirrer, an external magnetic stirrer or a user-controlled stirrer uncontrolled by the titrator (custom).

  • Page 56: Language

    GENERAL OPTIONS Language Select an available language. Estimated Cell Volume This screen allows the user to enter the estimated volume of solution in the titration beaker. Titrant Database This screen allows the user to store information about all of the titrants available for use, including the titrant name and Standardization information.

  • Page 57: Standard Database

    GENERAL OPTIONS 4.8 Standard Database This screen allows the user to store information about all of the standards available for use, including the standard name and concentration. The standard for the currently-selected method can not be modified from this screen. For details on the full functionality of the database, see section 5.5.11.
  • Page 58 The status of the transfer (“successful” / ”unsuccessful”) and the file name of the currently processed file are displayed during copying or deleting. Note: The saved files will be stored on the USB Key in the HI 903 folder, as follows: - Methods: USB Drive: \ HI 903 \ Methods \ *.mtd...

  • Page 59: Restore Files From Usb Storage Device

    Note: In order to restore files from USB Key, please ensure that the methods and/or reports you wish to transfer to the titrator are in the correct folder: - Methods: USB: \ Drive \ HI 903 \ Methods \ *.mtd - Reports: USB: \ Drive \ HI 903 \ Reports \ *.rpt...

  • Page 60: Usb Link With

    GENERAL OPTIONS 4.11 USB Link with PC The USB Link feature is useful to transfer methods/reports directly to/from a PC. To use this feature, connect the USB cable to the labeled connector on rear of titrator and connect to a PC with HI900PC Application installed.

  • Page 61: Setup Balance Interface

    GENERAL OPTIONS Disconnect the KF electrode, then connect the HI900941 calibration key to the electrode input (BNC connector). Depending on which parameters you want to check, follow the indications below: Checking the mV input accuracy: Set the multimeter to mV mode. If necessary, switch the calibration key to mV mode by pressing the red button.

  • Page 62: Printer Mode

    GENERAL OPTIONS Configure the settings on the titrator Balance Configuration menu to match the settings for your particular balance (baud rate, data bits, parity, stop bit number, request command syntax). It may be necessary to change settings on your balance. Users should consult their balance instruction manual.

  • Page 63: Reset To Default Settings

    GENERAL OPTIONS 4.15 Reset to Default Settings This option restores the manufacturer settings. Note: Please be careful!!! This will also delete all the user created methods, reports and restore all manufacturer settings such as titrator configuration, standard method parameters, etc. 4.16 Update Software This screen allows the user to update the titrator software from a USB storage device con-...
  • Page 65 METHODS Chapter 5. Contents METHODS ....................5 - 3 Selecting Methods ................5 - 3 Standard Methods ................. 5 - 4 5.2.1 Upgrading Standard Methods ............... 5 - 4 5.2.2 Deleting Standard Methods ................5 - 4 5.2.3 Restoring the Standard Methods to the Manufacturer’s Settings ....... 5 - 5 User Methods ..................
  • Page 66 METHODS 5.5.11.3 Concentration Unit ..................5 - 16 5.5.11.4 Water Content ....................5 - 16 5.5.11.5 Standard Size ....................5 - 16 5.5.12 Titrant ....................... 5 - 16 5.5.12.1 Titrant Name ....................5 - 17 5.5.12.2 Titrant Type ....................5 - 17 5.5.12.3 Nominal Titrant Concentration ................

  • Page 67: Methods

    METHODS METHODS All of the parameters required to complete an analysis are grouped into a method. The titrator is supplied with a pack of standard methods. Standard and user methods can be upgraded, stored or deleted by connecting the titrator to a PC using the HI900PC application or a USB storage device.

  • Page 68: Standard Methods

    METHODS Standard Methods The standard methods were developed for the most common types of analysis. Also, the standard methods can be used as a model to create new user methods. Only specific method parameters can be modified by the user (see Section 5.5, Method Op- tions section).

  • Page 69: Restoring The Standard Methods To The Manufacturer's Settings

    METHODS 5.2.3 Restoring the Standard Methods to the Manufacturer Settings You can restore the standard method to the manufacturer setting by highlighting a standard method and pressing 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.

  • Page 70: Deleting User Methods

    METHODS Note: Only a limited number of user methods can be generated. The titrator can hold 100 methods (standard and user). When it is reached, a warning message will be displayed. 5.3.2 Deleting User Methods To remove a user method, press (when available).

  • Page 71: Method Options

    METHODS Save method: After making modifications highlight Save Method and press After making modifications, press and select Save Method to keep the changes. Method Options 5.5.1 Naming the User Method This option allows you to enter a name for the new method (up to 24 characters). Use the arrow keys to navigate through the character table.

  • Page 72: Method Revision

    METHODS 5.5.2 Method Revision This option allows you to enter a string representing the current method revision. The revision string format should be “X.Y”, where X and Y are numerical digits. 5.5.3 Method Type Method type is a parameter listed in each method. In order to conduct a titration the user has to choose between water determination in the sample (Sample Analysis) or determination of titrant concentration (Titrant Standardization).

  • Page 73: Predispensing Amount

    METHODS 5.5.4 Predispensing Amount The titration time can be shortened by adding a large fraction of the titrant at the start of the analysis, if the approximate water content of the sample is known. The predispensing amount can be set to deliver between 1 and 90% of the titrant required to reach the end point.

  • Page 74: Stirring Speed

    METHODS 5.5.6 Stirring Speed The stirring speed can be set between 200 and 2000 RPM with a resolution of 100 RPM. The stirrer will remain on, as long as the method is active. The speed can be adjusted at any time by using the keys when the stirrer is running.

  • Page 75: Drift Entry

    METHODS 5.5.8 Drift Entry Allows the user to choose the drift entry mode that 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 user enters the estimated drift value.

  • Page 76: Solvent Name

    METHODS 5.5.9 Solvent Name The user can enter a name for the solvent (up to 15 characters). Use the arrow keys to navigate through the character table. Press to add the highlighted character to the solvent name. 5.5.10 Sample Parameters ( Sample Analysis mode only) This screen allows the user to access and configure the specific sample parameters.

  • Page 77: Sample Determination

    METHODS 5.5.10.1 Sample Determination This screen allows the user to select the sample determination mode. Normal sample determination is performed through direct titration of samples that are soluble in solvent or are finely divided and have homogeneous distribution in water. External extraction is a method for the preparation of insoluble samples that require an external water extraction.

  • Page 78: Sample Type

    METHODS 5.5.10.3 Sample Type This option allows the user to select the type of the sample: mass, volume or pieces. This information is used to determine the appropriate sample size required by the titration prior to analysis. 5.5.10.4 Sample Size This option allows the user to enter the sample size.

  • Page 79: Standard ( Titrant Standardization Mode Only)

    METHODS 5.5.10.5 External Solvent Size ( External Dissolution/Extraction Determination Modes Only). Enter the mass of the solvent used for external dissolution or extraction of the sample. Weigh the solvent after determining the solvent water content but before adding sample to the solvent External Dissolution/Extraction Modes Only).

  • Page 80: Standard Name

    METHODS 5.5.11.1 Standard Name This option allows the user to edit the name of the standard. 5.5.11.2 Standard Type The user can select the type of the standard: Mass or Volume. 5.5.11.3 Concentration Unit The concentration unit can be selected: %[W/W], ppm, mg/g, mg/mL. 5.5.11.4 Water Content The concentration of the standard can be entered (content of water in the selected unit).

  • Page 81: Titrant

    METHODS 5.5.13 Titrant The user can access the Karl Fischer titrant database and customize related parameters. Using the keys, highlight the titrant from the existing list and press choose it. Press to create a new titrant. Titrant Press to remove the titrant from the list. Press to edit the titrant parameters.

  • Page 82: Titrant Name

    METHODS 5.5.13.1 Titrant Name The user can edit the name for the titrant. 5.5.13.2 Titrant Type The user can select the type of titrant. 5.5.13.3 Nominal Titrant Concentration The user can enter the titrant concentration. 5.5.13.4 Standardized Titrant Concentration The user can manually enter the exact titrant concentration. 5-18...

  • Page 83: Titrant Age Reminder

    METHODS 5.5.13.5 Titrant Age Reminder The user can set a reminder that a verification of the titrant concentration is necessary. When the set reminder period has expired, a warning message will be displayed on the main screen. The reminder period will reset once the titrant is restandardized or the set time is modified.

  • Page 84: Start Mode

    METHODS 5.5.14.1 Start Mode The user can select the starting mode for the titration. In Cautious mode, the titrant dosing begins with the minimum dose in order to prevent over-titration. In Normal mode, the titrant dosing begins with the median value between the minimum and maximum (i.e. minimum dose 5 µL, maximum dose 25 µL, first dose will be 15 µL).

  • Page 85: Standby Duration

    The user can set the standby period up to 23 hours and 59 minutes. 5.5.14.4 Imposed Current The HI 903 uses a bivoltametric electrode system. During a titration, the titrator monitors the voltage required to maintain a constant polarization current (imposed current).

  • Page 86: Dosing Parameters

    METHODS 5.5.14.5 Dosing Parameters The user can set the minimum and maximum volume of titrant / dose. The titrant min and max dose values are determined by the type of reagent, reagent concentra- tion and the expected content of water in the sample. Correct determination of these values is necessary in order to prevent over-titration and ensure the highest possible accuracy.

  • Page 87: End Point Value

    METHODS 5.5.14.7 End Point Value This option defines the mV value at which the titration equivalence point (endpoint) has been reached. The pre-titration is completed when the mV is under the endpoint value, for a user defined period of time (see Section 5.5.14.4, Endpoint Stability Time ). The mV value can be set from 5.0 to 600.0 mV.

  • Page 88: Flow Rate

    METHODS 5.5.14.9 Flow Rate The flow rate for the dosing system can be set by the user in an interval of 0.1 to two times the burette volume: 0.1 to 10 mL/min for a 5 mL burette Note: The titrator will automatically detect the burette size and display the correct high limit volume.

  • Page 89: Maximum Duration

    METHODS 5.5.15.1 Maximum Duration Specify the maximum time a titration is allowed to run. Once this point is reached the titration will be terminated even if the end point is not reached. The time can be set from 10 to 3600 seconds. 5.5.15.2 Maximum Titrant Volume The maximum titrant volume used in the titration must be set according to the analysis.

  • Page 90: Termination Criterion

    METHODS 5.5.15.3 Termination Criterion This screen allows the user to set the titration termination criterion. mV End Point The titration is terminated when the potential remains below a set mV value for a specified period of time (see Section 5.5.14.4, End Point Stability Time).

  • Page 91: Result Unit

    METHODS 5.5.16 Result Unit The titrator provides the results based on the selected units. 5.6 Printing To print method parameters, press from the main screen, then If no printer is connected to the dedicated socket, or if the printer is offline, an error message will appear on the display (see Section 8.3.3, Connecting a Printer for information about connecting a printer to the titrator).
  • Page 93 TITRA TITRA TION TION TITRA TITRA TION TITRA TION TION Chapter 6. Contents TITRATION ................... 6 - 3 Idle ......................6 - 3 Pre-titration..................6 - 3 Drift Analysis ..................6 - 4 Standby ....................6 - 5 Sample Analysis ..................6 - 6 Titrant Standardization ................

  • Page 94: Titration

    TITRA TITRA TION TION TITRA TITRA TITRA TION TION TION...

  • Page 95: Idle

    TITRATION Idle The titrator first enters Idle mode when it is switched on. All of the HI 903’s software features and adjustable parameters can be accessed from the Idle state. This includes all of the user- adjustable method parameters, solvent handling system, file transfers, calibration checks, soft- ware upgrades, options for interface with PC and accessories as well as burette options.

  • Page 96: Drift Analysis

    ‘dryness’ of the solvent over the course of a minute. The rate at which water leaks into the cell is then calculated and reported by the HI 903 in units of µg/min. The HI 903 uses the drift rate determined during this state to automatically subtract the quantity of water which leaks into the cell during a titration from titration results.

  • Page 97: Standby

    TION TION Standby After the drift rate has been determined, the HI 903 moves into Standby mode. In standby mode the dryness of the titration cell is maintained and the drift rate is continuously moni- tored and updated. From Standby mode a sample analysis, titrant standardization or drift rate logging session can be launched as well as method selection, customization of method parameters, and general options (external keyboard only, by pressing <<Home>>).

  • Page 98: Sample Analysis

    TITRA TITRA TION TITRA TION TION TION TITRA TITRA TION Sample Analysis While in Standby mode, press Note: If the drift value is zero a warning message appears to inform the user that the solvent may be overtitrated. The user can choose to continue the titration by pressing or to return to Standby mode by pressing in order to wait until the drift is stabilized at a higher value.
  • Page 99 TITRA TITRA TITRA TION TION TION TION TITRA TITRA TION Manual Entering Follow the steps below: Sample size by mass : 1. Measure the mass of the sample in a weigh boat or syringe. 2. Slide the sample plug up out of the vessel top to open the sample port, or insert the syringe needle through the septum.
  • Page 100 TITRA TITRA TION TITRA TION TION TION TITRA TITRA TION Automatic Mass Acquisition from Analytical Balance It is available only for Sample Mass and Sample Volume types. The sample size can be automatically acquired from the balance when connected to the titrator using the RS232 interface.
  • Page 101 TITRA TITRA TITRA TION TION TION TION TITRA TITRA TION The titrator returns to the previous screen and the sample size is automatically updated. Now the analysis can be started. Start Analysis Press to begin analysis. Suspend Titration While the titration is in progress, you can temporarily stop it by pressing .
  • Page 102 TITRA TITRA TION TITRA TION TION TION TITRA TITRA TION Viewing the Titration Curve During a titration, the titration curve can be displayed on the Titration Graph screen, by pressing . The titration ID report is also displayed inside the graph window. Press to stop the titration manually and return to Idle mode.

  • Page 103: Titrant Standardization

    TITRA TITRA TION TION TITRA TITRA TION TITRA TION TION Averaging Sample Analysis Results By pressing , results will be added to the Sample Analysis History in order to obtain an average of titration results. Use the keys to scroll the concentration results list. to choose the sample concentration results that will be used for averaging.
  • Page 104 TITRA TITRA TION TITRA TION TION TION TITRA TITRA TION Adding the standard: The user must add the standard into the beaker and enter the standard size. The units of sample size are determined by the method setting. Follow the same procedure as for adding samples ( see Section 6.5, Sample Analysis ) Start Standardization Press to begin standardization.
  • Page 105 TITRA TITRA TION TION TITRA TITRA TION TITRA TION TION Averaging Titrant Standardization Results By pressing results can be added to the sample analysis history in order to obtain an average of titrant concentration. Use the keys to scroll the concentration results list. to choose the titrant concentration results that will be used for averaging.
  • Page 106 TITRA TITRA TION TION TITRA TITRA TITRA TION TION TION 6-14...
  • Page 107 AUXILIARY FUNCTIONS AUXILIARY FUNCTIONS AUXILIARY FUNCTIONS AUXILIARY FUNCTIONS AUXILIARY FUNCTIONS Chapter 7. Contents AUXILIARY FUNCTIONS ................ 7 - 3 7.1 Air Pump ....................7 - 3 7.1.1 Filling the Beaker ..................7 - 3 7.1.2 Emptying the Beaker................... 7 - 3 7.2 Burette ....................

  • Page 108: Auxiliary Functions

    AUXILIARY FUNCTIONS AUXILIARY FUNCTIONS AUXILIARY FUNCTIONS AUXILIARY FUNCTIONS AUXILIARY FUNCTIONS...

  • Page 109: Air Pump

    Fill button and deactivate the air pump with the option key. 3. The HI 903 will prompt the user to verify that the titration cell has been filled to the ‘min’ line (approx. 50 mL). to return to Idle screen.

  • Page 110: Burette

    AUXILIARY FUNCTIONS AUXILIARY FUNCTIONS AUXILIARY FUNCTIONS AUXILIARY FUNCTIONS AUXILIARY FUNCTIONS Burette To access the Burette screen, press from the Idle screen. Highlight the desired option and then press Note: Do not perform burette functions with solvent below the “Min” sign. Doing so could spray titrant on the beaker top or other components.

  • Page 111: Rinse Tip

    AUXILIARY FUNCTIONS AUXILIARY FUNCTIONS AUXILIARY FUNCTIONS AUXILIARY FUNCTIONS AUXILIARY FUNCTIONS To prime the burette, select Prime Burette from the Burette screen. Enter the number of rinses and press The number of burette rinses can be set between 1 and 5 (we recommend at least three rinses to assure that the air bubbles are completely removed).

  • Page 112: Purge Burette

    AUXILIARY FUNCTIONS AUXILIARY FUNCTIONS AUXILIARY FUNCTIONS AUXILIARY FUNCTIONS AUXILIARY FUNCTIONS The manual dispense volume must be between the limits shown below: 0.001 to 4.500 mL for a 5-mL burette 7.2.4 Purge Burette This option allows the burette to be emptied before cleaning and/or storing. Note: Before starting this operation, remove the aspiration tube from the titrant bottle.

  • Page 113: Results

    AUXILIARY FUNCTIONS AUXILIARY FUNCTIONS AUXILIARY FUNCTIONS AUXILIARY FUNCTIONS AUXILIARY FUNCTIONS Results To access the “Data Parameters” screen, press button. From the Data Parameters screen you can access the following options: 7.4.1 Review Last Titration Report The last titration report can be reviewed. The titration graph can be reviewed by selecting The information seen in the report is based on the selections made in the Setup Titration Report screen.

  • Page 114: Review Available Reports

    AUXILIARY FUNCTIONS AUXILIARY FUNCTIONS AUXILIARY FUNCTIONS AUXILIARY FUNCTIONS AUXILIARY FUNCTIONS 7.4.2 Review Available Reports Up to 100 reports can be saved on the titrator. To view one of the saved reports highlight a report and then press Report All of the saved reports can be reviewed and printed. The report contains only the information selected in the Setup Titration Report screens during report generation.

  • Page 115: Meter Information

    AUXILIARY FUNCTIONS AUXILIARY FUNCTIONS AUXILIARY FUNCTIONS AUXILIARY FUNCTIONS AUXILIARY FUNCTIONS Company Name: Allows the company name to be recorded in each report. Operator Name Allows the operator name to be recorded in each report. Electrode Name Allows the electrode name to be recorded in each report. Fields 1, 2, 3 Allows any additional information to be recorded in each report.

  • Page 116: Setup Titration Report

    AUXILIARY FUNCTIONS AUXILIARY FUNCTIONS AUXILIARY FUNCTIONS AUXILIARY FUNCTIONS AUXILIARY FUNCTIONS 7.4.5 Setup Titration Report Customize a unique report to record the titration results. An asterisk means that it will be included in the titration report. 7-10...
  • Page 117 MAINTENANCE, PERIPHERALS Chapter 8. Contents MAINTENANCE, PERIPHERALS .............8 - 3 Burette Maintenance ................8 - 3 8.1.1 Burette Assembly ..................8 - 3 8.1.2 Changing the Burette .................8 - 3 8.1.3 Disassembling the Dispensing Tube and Aspiration Tube ....... 8 - 4 8.1.4 Assembling the Dispensing Tube and Aspiration Tube ........

  • Page 118: Maintenance, Peripherals

    MAINTENANCE, PERIPHERALS...

  • Page 119: Burette Maintenance

    MAINTENANCE, PERIPHERALS MAINTENANCE, PERIPHERALS The 5-mL burette included with the titrator exceeds the ISO 8655 standard for the accurate delivery of liquids by a motor-driven piston burette. Burette Maintenance 8.1.1 Burette Assembly The burette is delivered with a 5-mL syringe inside and with all the accessories mounted (see Section 2.

  • Page 120: Disassembling The Dispensing Tube And Aspiration Tube

    MAINTENANCE, PERIPHERALS 8.1.3 Disassembling the Dispensing Tube and Aspiration Tube Both the aspiration and the dispensing tubes have a fitting and a tube protector. The aspiration tube will be mounted in the left side and the dispensing tube will be mounted in the right side of the burette.

  • Page 121: Cleaning The Burette

    MAINTENANCE, PERIPHERALS 8.1.5 Cleaning the Burette To clean the burette, follow these steps: • If the burette is filled with titrant, remove the aspiration tube from the titrant bottle and purge burette ( see Section 7.2.4, Purge Burette • Insert the aspiration tube into the Karl Fischer solvent. •...
  • Page 122 MAINTENANCE, PERIPHERALS Warning: Avoid contact with the titrant with bare hands. Avoid spilling titrant. Clean the external side of the syringe and piston to remove aggressive chemicals. Do not touch the Teflon part of the piston or internal walls of the burette with bare hands or greasy materials.

  • Page 123: Burette Preparation (Filling With Titrant)

    MAINTENANCE, PERIPHERALS 8.1.6 Burette Preparation (Filling with Titrant) Before starting a titration, the burette must be properly filled with titrant in order to obtain an accurate and repeatable result. To fill the burette, follow the next steps and recommenda- tions: •...

  • Page 124: Probe Maintenance

    MAINTENANCE, PERIPHERALS Probe Maintenance Proper probe maintenance is crucial for reliable measurements and extending the life of the probe. The frequency of maintenance will depend largely on the type of samples that are analyzed. Maintenance may be required if any of the following are observed: ·...

  • Page 125: Fuse Replacement

    MAINTENANCE, PERIPHERALS Fuse Replacement To replace the fuses, follow these steps: • Turn off the titrator. • Remove the power cord from the power connector located on the rear side of the titrator case. • With a screw driver open the fuse holder cover located at the rear of the Titrator. •...

  • Page 126: Connecting An External Display

    MAINTENANCE, PERIPHERALS 8.4.1 Connecting an External Display The information shown on the titrator display can be viewed also on a Standard VGA display connected with a 15-pin cable, as presented below. Connect the external display to the display socket. Turn on the titrator and then the external display. 8.4.2 Connecting an External PC Keyboard This connection allows you to use an external PS/2 PC Keyboard in addition to titrator’s...
  • Page 127 MAINTENANCE, PERIPHERALS (United States 101) Titrator Keypad Function Key F-1 Function Key F-2 Function Key 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)

  • Page 128: Connecting A Printer

    MAINTENANCE, PERIPHERALS 8.4.3 Connecting a Printer A variety of parallel printers can be connected to the parallel port of the titrator using a standard DB25–pin cable. Warning:The titrator and the external printer must both be OFF before they are connected. Connect the external printer to the standard 25–pin Socket.
  • Page 129 METHODS OPTIMIZATION Chapter 9. Contents OPTIMIZATION ..................9 - 3 Titrator Settings ................... 9 - 3 9.1.1 Control Parameters..................9 - 3 9.1.1.1 Endpoint Potential and Polarization Current ............9 - 3 9.1.1.2 Dosing Parameters ..................9 - 4 9.1.1.2.1 Minimum Dose ..................9 - 4 9.1.1.2.2 Maximum Dose ..................
  • Page 130 METHODS OPTIMIZATION 9.2.4 Liquid Samples ..................9 - 1 1 9.2.5 Sample Preparation Techniques ..............9 - 1 2 9.2.5.1 Internal Extractions ..................9 - 1 2 9.2.5.2 Dilutions ......................9 - 1 2 9.2.5.3 External Dissolution ..................9 - 1 3 9.2.5.4 External Extractions ..................9 - 1 3 9.2.5.5 Homogenization ....................9 - 1 4 9.2.5.6 Heating ......................9 - 1 4...

  • Page 131: Optimization

    During a titration, no excess iodine is present. In order to maintain the set polarization current the HI 903 must apply a relatively large voltage across the pins of the electrode. At the endpoint of the titration, the amount of iodine added is equal to the amount of water from the sample.

  • Page 132: Dosing Parameters

    The table that follows correlates endpoint potential ranges for each of the possible polarization current settings of the HI 903. The suggested endpoints below are applicable for reagents formulated with methanol. Endpoint potentials should be increased by 20 to 25% when...

  • Page 133: Timed Increment

    HI 903 as an approaching endpoint. This will in turn result in the dynamic dosing algorithm reducing the dose size until the excess iodine has time to react. The reduced dose size effectively interrupts the titration and adds considerable time to the titration duration.

  • Page 134: Start Mode

    METHODS OPTIMIZATION 9.1.1.4 Start Mode The HI 903 can be set to either normal or cautious start mode. The cautious start feature is designed to prevent the accidental over-titration of a sample with very low water content. In cautious start mode, the HI 903 starts a titration using the minimum dose size specified by the user rather than starting with half of the maximum dose size as with normal start mode.

  • Page 135: Relative Drift Stop

    Under this criteria a titration reaches an endpoint successfully when the HI 903 titrates all of the water introduced with the sample and maintains a drift rate which is equal to the sum of the initial drift (drift rate when the titration was initiated) and the set ‘relative drift stop’...

  • Page 136: Method Options

    9.1.3.3 Stirring Speed The HI 903’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 is rotating at the speed set by the user.

  • Page 137: The Sample

    METHODS OPTIMIZATION The Sample 9.2.1 Proper Sampling Procedure Proper sampling is essential for accurately determining the water content of bulk materials, particularly with non-homogeneous samples. Many standard methods detail instructions to ensure proper sampling. As a general rule, the following guidelines should be followed: 1.

  • Page 138: Solid Samples

    Solid samples are added to the titration cell by removing the sample plug. The quantity of solid sample added can be entered into the HI 903 as a mass or by number of pieces if, for example, pills are to be analyzed.
  • Page 139 13. Enter the calculated mass of the sample into the HI 903. 14. Start titration using the option key ‘start analysis’ from the add sample screen.
  • Page 140 The steps required for the most common sample preparation techniques are outlined below. For detailed application-specific instructions, consult the instructions included with applicable standard methods. The HI 903 provides options for the automatic calculation of samples prepared normally, using external extraction and external dissolution. 9.2.5.1 Internal Extractions Internal extractions are carried out using the ‘normal’...
  • Page 141 Sample preparation and choice of solvent or solvent mixture is sample specific. Consult an applicable standard method for procedural details. The HI 903 will conduct the necessary calculations automatically when ‘external dissolution’ is selected from the sample type menu. 9.2.5.4 External Extraction External extraction is recommended for insoluble solid samples which release water slowly.

  • Page 142: Homogenization

    METHODS OPTIMIZATION 6. Facilitate extraction by shaking the solution or placing the solution on a stirring plate or in a sonicator. 7. Allow the insoluble portion of the sample to settle to the bottom of the extraction bottle. 8. Titrate an appropriately sized sample of the supernatant (solvent above the settled solid sample).

  • Page 143: Karl Fischer Reagent System

    METHODS OPTIMIZATION Karl Fischer Reagent System A wide variety of Karl Fischer reagents exist on the market today, each designed and formulated for specific sample matrices and titration conditions. Karl Fischer reagent systems consist of a solvent and a titrant. The solvent is the liquid to which the sample is added in the reaction vessel.

  • Page 144: Choosing And Modifying A Solvent

    METHODS OPTIMIZATION proportional to carbonyl chain lengths. The formation of acetals and ketals is also dependent on the type of alcohol included in the solvent. As the chain length of an alcohol’s alkyl or substituted alkyl group increases, the alcohol’s reactivity toward ketones and aldehydes decreases (i.e.

  • Page 145: Standardizing The Titrant

    2. Select the appropriate standardization method included with the HI 903. Using a Sodium Tartrate Dihydrate Standard: 3. Back-weigh between 30 and 200 mg of standard. Be sure that the salt is a high quality standard, which has been stored properly and exists as a fine, free flowing powder.
  • Page 146 METHODS OPTIMIZATION 5. Review the set of results on the ‘average results’ statistics screen. The titrant concentration should be updated with the averaged results as long as there is not excessive variability between standardization results. 9-18...
  • Page 147 APPENDIX 1 Appendix 1. Contents TECHNICAL SPECIFICATIONS .............. A1-3 A1-1...
  • Page 148 APPENDIX 1 A1-2...
  • Page 149 APPENDIX 1 TECHNICAL SPECIFICATIONS Range 100 ppm to 100% Resolution 1 ppm to (0.0001%) Result Units %, ppm, mg/g, g/g, mg, g, mg/mL, g/mL, mg/pc, g/pc Sample Type Liquid or Solid Determination Pre-Titration Conditioning Automatic Background Drift Correction Automatic or User Selectable Value Endpoint Criteria Fixed mV persistence, Relative drift stop or Absolute drift stop...
  • Page 150 Alphanumeric text can be entered using an optional PS/2 keyboard Graphic Display 5.7” (320 x 240 Pixel) Color LCD Power Supply HI 903-01: 115 VAC, 50-60 Hz HI 903-02: 230 VAC, 50-60 Hz Power Draw HI 903-01: 0.2 Amps HI 903-02: 0.1 Amps...
  • Page 151 APPENDIX 2 Appendix 2. Recommended Reagents RECOMMENDED REAGENTS ..............A2-3 A2.1 Titrants ....................A2-3 A2.1.1 1-component Titrants ................A 2 - 3 A2.1.2 2-component Titrants................A 2 - 3 A2.2 Solvents ....................A 2 - 3 A2.2.1 1-component Solvents ................A 2 - 3 A2.2.2 1-component Solvents ................
  • Page 153 APPENDIX 2 A2 RECOMMENDED REAGENTS A2.1 Titrants A2.1.1 1-component Titrants Sigma-Aldrich® 34805 HYDRANAL® Composite 5 34806 HYDRANAL® Composite 2 34816 HYDRANAL® Composite 5K 34827 HYDRANAL® Composite 1 GFS Chemicals® 1600 WaterMark® Pyridine-Free Single Solution, 5 mg/mL 1601 WaterMark® Pyridine-Free Single Solution, 2 mg/mL J.T.
  • Page 154 APPENDIX 2 A2.2.2 2-component Solvents GFS Chemicals® 1609 WaterMark® Solvent, Methanol-Free 1610 WaterMark® Solvent, General Purpose J.T. Baker® 8855 HYDRA-POINT™ Solvent G A2.3 Standards Sigma-Aldrich® 34803 HYDRANAL® Standard Sodium Tartrate Dihydrate 34828 HYDRANAL® Water Standard 1.00 34847 HYDRANAL® Water Standard 0.10 34849 HYDRANAL®...
  • Page 155 APPENDIX 3 Appendix 3. Accesories TITRATOR COMPONENTS ..............A3-3 A3-1...
  • Page 157 APPENDIX 3 TITRATOR COMPONENTS HI900527 Septum, 5pcs HI900528 Solvent Port Plugs, 2pcs HI900530 HI900520 Titrant Bottle Top Beaker Assembly Assembly HI900531 Solvent/Waste Bottle Top Assembly HI900532 HI900522 Desiccant Cartridge for Beaker for HI903 Beaker or Titrant HI900523 Dispensing tip, 2pcs A3-3...
  • Page 158 2 x Tubing for Solvent/ Waste Handling HI900536 2 x Tubing for Air Pump HI900550 Desiccant, 250 g HI900810 Manual (English) for HI 903 HI900903U PC Application on USB Flash Drive HI900941 Calibration Key HI900942 Tool for Burette Cap Removal...
  • Page 159 GENERAL APPLICATIONS BROCHURE HI 903 KARL FISCHER VOLUMETRIC TITRATOR Revision 1.00...
  • Page 162 Method ID: HI8001EN 5.0 mg/mL Titrant Standardization using a Liquid Water Standard for one-component titrant Results: Titration Report Method Name: Stdz 5mg/mL w/ water Std. Time & Date: 12:00 Jan 1, 2011 Standard Size: 1.0000 g Standard Conc.: 10.0000 mg/g Drift Value: 5.4 ug/min End Point Volume:...
  • Page 164 Method ID: HI8002EN 2.0 mg/mL Titrant Standardization using a Liquid Water Standard for one-component titrant Results: Titration Report Method Name: Stdz 2mg/mL w/ water Std. Time & Date: 12:00 Jan 1, 2011 Standard Size: 2.0000 g Standard Conc.: 1.0000 mg/g Drift Value: 5.0 ug/min End Point Volume:...
  • Page 166 Method ID: HI8003EN 1.0 mg/mL Titrant Standardization using a Liquid Water Standard for one-component titrant Results: Titration Report Method Name: Stdz 1mg/mL w/ water Std. Time & Date: 12:00 Jan 1, 2011 Standard Size: 2.0000 g Standard Conc.: 1.0000 mg/g Drift Value: 5.0 ug/min End Point Volume:...
  • Page 168 Method ID: HI8011EN 5.0 mg/mL Titrant Standardization using Disodium Tartrate Dihydrate for one-component titrant Results: Titration Report Method Name: Stdz 5mg/mL w/ Tartrate Time & Date: 12:00 Jan 1, 2011 Standard Size: 0.1000 g Standard Conc.: 15.66 % Drift Value: 4.0 ug/min End Point Volume: 3.1185 mL...
  • Page 170 Method ID: HI8101EN Moisture Determination in Dairy Cream Results: Titration Report Method Name: Moisture in Dairy Cream Time & Date: 12:00 Jan 01, 2011 Sample Size: 0.0241 g Std. Titrant Conc.: 5.0000 mg/mL Drift Value: 4.7 ug/min End Point Volume: 3.4567 mL Result: 71.5481 %...
  • Page 172 Method ID: HI8102EN Moisture Determination in Milk Results: Titration Report Method Name: Moisture in Milk Time & Date: 12:00 Jan 01, 2011 Sample Size: 0.0188 g Std. Titrant Conc.: 5.0000 mg/mL Drift Value: 4.5 ug/min End Point Volume: 3.2614 mL Result: 86.5886 % Titration Duration:...
  • Page 176 Method ID: HI8104EN Surface Moisture Determination on White Sugar Results: Titration Report Method Name: Surface Moisture - Sugar Time & Date: 12:00 Jan 1, 2011 Sample Size: 7.5231 g Std. Titrant Conc.: 1.0000 mg/mL Drift Value: 5.7 ug/min End Point Volume: 2.4292 mL Result: 319 ppm...
  • Page 178 Method ID: HI8105EN Moisture Determination in Cooking Oil Results: Titration Report Method Name: Moisture in Cooking Oil Time & Date: 12:00 Jan 1, 2011 Sample Size: 4.0296 g Std. Titrant Conc.: 1.0000 mg/mL Drift Value: 3.4 ug/min End Point Volume: 2.6808 mL Result: 660 ppm...
  • Page 180 Method ID: HI8106EN Moisture Determination in Butter by external dissolution Method Parameters: Results: Name: Moisture in Butter Titration Report Method Revision: Method Name: Moisture in Butter Type: Sample Analysis Time & Date: 12:00 Jan 01, 2011 Predispensing Amount: None Sample Size: 0.7841 g Pre-Analysis Stir Time: 10 Sec...
  • Page 182 Method ID: HI8107EN Moisture Determination in Margarine by external dissolution Method Parameters: Results: Name: Moisture in Margarine Titration Report Method Revision: Method Name: Moisture in Margarine Type: Sample Analysis Time & Date: 12:00 Jan 01, 2011 Predispensing Amount: None Sample Size: 0.7402 g Pre-Analysis Stir Time: 10 Sec...
  • Page 184 Method ID: HI8108EN Moisture Determination in Mayonnaise by external extraction Method Parameters: Results: Name: Moisture in Mayonnaise Titration Report Method Revision: Method Name: Moisture in Mayonnaise Type: Sample Analysis Time & Date: 12:00 Jan 01, 2011 Predispensing Amount: None Sample Size: 0.7500 g Pre-Analysis Stir Time: 10 Sec...
  • Page 186 Method ID: HI8201EN Moisture Determination in Shampoo Results: Titration Report Method Name: Moisture in Shampoo Time & Date: 12:00 Jan 1, 2011 Sample Size: 0.0200 g Std. Titrant Conc.: 5.0000 mg/mL Drift Value: 5.4 ug/min End Point Volume: 3.2010 mL Result: 79.9207 % Titration Duration:...
  • Page 188 Method ID: HI8202EN Moisture Determination in Hand Cream Results: Titration Report Method Name: Moisture Hand Cream Time & Date: 12:00 Jan 1, 2011 Sample Size: 0.0244 g Std. Titrant Conc.: 5.0000 mg/mL Drift Value: 5.4 ug/min End Point Volume: 2.6925 mL Result: 67.3125 % Titration Duration:...
  • Page 190 Method ID: HI8301EN Moisture Determination in Solvent with 5 mg/mL Titrant (One-Comp.) for external dissolution or extraction Results: Titration Report Method Name: Solvent w/ 5mg/mL 1-comp. Time & Date: 12:00 Jan 01, 2011 Sample Size: 0.9580 g Std. Titrant Conc.: 5.0000 mg/mL Drift Value: 4.0 ug/min...
  • Page 191 TITRATION THEORY TITRATION THEORY Principles HI 903 KARL FISCHER VOLUMETRIC TITRATOR Revision 1.0...
  • Page 192 TITRATION THEORY...
  • Page 193 TITRATION THEORY Contents GENERAL REVIEW OF TITRATION THEORY ................5 Introduction to Titrations ....................5 Uses of Titrations ......................5 Advantages and Disadvantages of Titrations ..............6 TYPES OF TITRATION ......................7 Titrations According to The Measurement Method ............. 7 2.1.1 Amperometric Titrations ......................
  • Page 194 TITRATION THEORY...

  • Page 195: General Review Of Titration Theory

    TITRATION THEORY GENERAL REVIEW OF TITRATION THEORY Introduction to Titrations A titration is a quantitative, volumetric procedure used in analytical chemistry to determine the concentration of an analyte (the species being measured) in solution. The concentration of the analyte is determined by slowly adding a titrant (reagent) to the solution. As the titrant is added, a chemical reaction occurs between the titrant and the analyte.

  • Page 196: Advantages And Disadvantages Of Titrations

    TITRATION THEORY Advantages and Disadvantages of Titrations Some advantages of titrations, as an analytical technique, are: • More precise results than many instrumental methods, such as measurement by electrode, the accuracy of the measurement is up to 0.1%; • Simple methods, reasonable capital costs, and easy training; •...

  • Page 197: Types Of Titration

    TITRATION THEORY TYPES OF TITRATIONS Titrations According to The Measurement Method 2.1.1 Amperometric Titrations An amperometric titration is performed by placing two electrodes (often a metal electrode and a reference electrode) into the sample solution and holding the potential of the metal electrode at a selected voltage.

  • Page 198: Spectrophotometric Titrations

    TITRATION THEORY electrode, are monitored to show the progress of the titration. Potentiometry is the measurement of a potential under conditions of zero current flow. The measured potential can then be used to determine the analytical quantity of interest, generally a component concentration of the analyte solution.

  • Page 199: Titrations According To The Reaction Type

    TITRATION THEORY Titrations According to The Reaction Type 2.2.1 Karl Fischer Titrations This method is based on a well-defined chemical reaction between water and the Karl Fischer reagent. The chemistry provides excellent specificity for water determination. The method can be used to determine free and bound water in a sample matrix. The Karl Fischer method is widely considered to produce the most rapid, accurate and reproducible results and has the largest detectable concentration range spanning 1 ppm to 100%.

  • Page 200: Visual Indication Of Karl Fischer Titrations

    TITRATION THEORY of reaction decreases and titration endpoint become increasingly difficult to reach. If the pH exceeds 8, side reactions begin to occur between iodine and hydroxide or methylate ions, changing the titration stoichiometry. While solvents not containing alcohols can be used for Karl Fischer analysis, they also have an effect on reaction stoichiometry.

  • Page 201: Acid-Base Titrations

    TITRATION THEORY Bivoltametric indication involves measuring the voltage required to maintain a constant current flow between electrode elements. A small direct or alternating current called a polarization current (I pol ) is applied between the electrode pins or rings and the resulting voltage is measured in order to monitor the titration progress.

  • Page 202: Argentometric Titrations

    TITRATION THEORY Figure 3 shows a traditional titration curve. The curve is obtained by plotting the pH value against the volume of NaOH added. Figure 3 2.2.3 Argentometric Titrations Argentometric titrations use silver (nitrate) as the titrant and are generally precipitation titrations, as many silver salts are insoluble.

  • Page 203: Ion Selective Titrations

    TITRATION THEORY titrant that binds strongly to it. Often these titrants contain EDTA or CDTA, polydentate ligands that form very stable coordination compounds with metal ions. The complexation reaction must be fast in order to be useful for direct titration. Some metal ions react too slowly with EDTA for a direct titration.

  • Page 204: Precipitation Titrations

    TITRATION THEORY carboxylic acids, enols, phenols, imides, sulfonic acids, and inorganic acids. Water or lower alcohols are suitable for titrating medium to strong acids (pK a less than 5). Titrating a weaker acid with a strong base titrant requires a solvent less acidic than water or ethanol/methanol. Solvents such as acetone, acetonitrile, t-butyl alcohol, dimethlyformamide, isopropanol and pyridine have been found to work well for acid-base titrations of strong, medium and weak acids/ bases.

  • Page 205: Titrations According To The Titration Sequence

    TITRATION THEORY Figure 6. Figure 7. oxidant reductant ratio. Visual indicators such as Ferrion are also available. The oxidized and reduced form of the indicator will have different colors and can be used to determine the end point. Various reductants can be determined by titrants with oxidants such as potassium permanganate, potassium chromate or iodine.
  • Page 206 TITRATION THEORY Figure 8.

  • Page 207: Introduction To Titration Apparatus And Typical Titration Procedure

    TITRATION THEORY INTRODUCTION TO TITRATION APPARATUS AND TYPICAL TITRATION PROCEDURE Manual Titration Apparatus required for manual titration include: • Volumetric Burette, for precisely controlled delivery of titrant to the reaction vessel; • An Erlenmeyer, or similar flask, that facilitates constant mixing or swirling required to ensure solution homogeneity;...

  • Page 208: Automatic Titration

    TITRATION THEORY Automatic Titration Automatic titrators are high-precision analytical instruments that deliver the titrant, monitor the physical change associated with the titration reaction, automatically stops at the endpoint and calculates the concentration of the analyte. Automatic titrators are best for repetitive titrations and high-accuracy analyses.

  • Page 209: Titration Results

    TITRATION THEORY TITRATION RESULTS Accuracy The factors most critical to achieving accurate results with the HI 900 titration systems are the concentration of the sample, size of the sample and having an optimized set of method parameters. Repeatability Repeatability, or the agreement between replicate determinations, is expressed quantitatively as the relative standard deviation (RSD).

  • Page 210: Dispensing Errors

    TITRATION THEORY 4.3.2.2 Dispensing Errors Incorrect dispensing due to: • Dead valve volume and leaking valve; • Inaccuracy in motor drive and gear lash/ backlash; • Poor burette/ piston seal; • Non-uniform diameter of burette glass cylinder; • Chemical incompatibility with tubing or bubble generation; •...

  • Page 211: Calculations

    TITRATION THEORY CALCULATIONS Equations Used in Volumetric Karl Fischer Titrations 5.1.1 Calculation of water content as % mass from samples measured by mass C sample Concentration of Sample (% w/w) V titrant Volume of Titrant (mL) Titer Titrant Titer (mg/mL) m sample Mass of Sample (g) 5.1.2 Calculation of water content as % mass from samples measured by volume...

  • Page 212: Calculation Of Water Content In External Dissolutions Samples

    TITRATION THEORY 5.1.5 Calculation of water content in External Dissolution Samples C sample Concentration of Sample (% w/w) m solvent Mass of Solvent (g) m sample Mass of Sample (g) C solution Water Content of Dissoluted Sample (w/w) C solvent Water Content of Solvent (w/w) 5.1.6 Calculation of water content in External Extraction Samples...

  • Page 213: Calculation Of Titer (Water Equivalent Of The Titrant) Using Water Standards

    TITRATION THEORY 5.1.9 Calculation of titer (water equivalent of the titrant) using water standards C titrant Titrant Titer (mg/mL) m sample Mass of Sample (g) C standard Water Content of Standard (mg/g) V titrant Volume of Titrant (mL) Equations Used in Titrations The main variables used in calculating a result from a titration are the sample volume, the concentration of the titrant, and the volume of titrant required to reach the equivalence point.

  • Page 214: Blank Titration

    TITRATION THEORY By Mass C titrant Titrant Concentration (N) m standard Mass of Standard (g) Ratio Equivalence ratio of titrant/standard (eq titrant/ mol standard) FW standard Formula Weight of the Standard (g/mol) V titrant Volume of Titrant (L) By Volume C titrant Concentration of titrant (N) V standard...

  • Page 215: Back Titration

    TITRATION THEORY       C sample1 Sample 1 Concentration (g/100g) C sample2 Sample 2 Concentration (g/100g) C sample3 Sample 3 Concentration (g/100g) V titrant 1 Volume of titrant required to reach the first end point (L) V titrant 2 Volume of titrant required to reach the second end point (L) V titrant 3...

  • Page 216: Glossary

    TITRATION THEORY 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 and base. Activity A physical property corresponding to the concentration of all ions in a solution. Elec- trodes respond to activity.
  • Page 217 TITRATION THEORY End point The point where a titration is stopped because a physical change in the solution has indicated a completed titration. Titration end points typically coincide with the equiva- lence point . A fixed value end point (pH or mV), can be used as well. The titration will stop at the desired point regardless if the titration is complete.
  • Page 218 TITRATION THEORY Neutralization A chemical reaction where an acid and a base react to form a neutral salt and water. Non-aqueous A solution that does not contain water. Non-aqueous Titration A titration that is preformed in non-aqueous solutions. Typically used to titrate very weak acid and bases to eliminate the leveling effect water has on all acids and bases dissolved in it.
  • Page 219 TITRATION THEORY Spectrophotometric Titration A titration in which the end point 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. Titration A quantitative, volumetric procedure used in analytical chemistry to determine the concentration of an analyte in solution.
  • Page 220 TITRATION THEORY...

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