Hanna Instruments HI 904 Uick Start Manual
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Hanna Instruments HI 904 Uick Start Manual

Karl fischer coulometric titrator
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QUICK START GUIDE
HI 904
KARL FISCHER
COULOMETRIC TITRATOR
Revision 1.0
www.hannainst.com
1

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  • Page 1 QUICK START GUIDE HI 904 KARL FISCHER COULOMETRIC TITRATOR Revision 1.0 www.hannainst.com...
  • Page 2 Dear customer, Congratulations on choosing a Hanna Instruments Product. This guide has been written for the HI 904 Karl Fischer Coulometric 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: Table Of Contents

    QUICK START GUIDE Contents 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 PERFORM THE FIRST TITRATION ..............10...
  • Page 4 QUICK START GUIDE...
  • Page 5 The HI 904 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. Never connect or disconnect the pump assemblies with the titrator turned on. 2. Always check that the reagent and waste bottles, as well as the titration vessel are properly assembled.

  • 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 904 Karl Fischer titrator can store up to 100 methods: these include up to 90 standard methods. Standard Methods Each titrator is supplied with a customized package of standard methods.

  • Page 10: Before Performing The First Titration

    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 vessel system is properly sealed against atmospheric moisture (the fittings and tubes are correctly mounted).
  • Page 11 QUICK START GUIDE Fill Titration Vessel with Reagent The titration vessel must be filled with reagent up to the MIN marker (about 75 mL): • Lower the reagent tube below the liquid level inside the reagent bottle. • From the Idle screen, press •...
  • Page 12 QUICK START GUIDE Liquid Samples: • Samples with low viscosity will be added using a syringe with needle (injection through the septum). • Weigh the syringe before and after injection in order to increase precision (back-weighing technique). Sample Volume Preparation Liquid samples with low viscosity can be added by volume.
  • Page 13 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. Titrated Water. 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 14 QUICK START GUIDE • The Review Result screen will be displayed. • Use the keys to display information related to the last titration performed. 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 15 HI904 - Titration Report Method Name: Moisture in Chloroform Time & Date: 15:15 Jul 28, 2013 Titration ID: KF_00003 Company Name: Hanna Instruments Operator Name: KF Technician Electrode Name: Probe 1 Field 1: Any text Field 2: Any text...
  • Page 16 QUICK START GUIDE Nr Titr Water[µg] Time 385.7 00:00:00 385.7 00:00:01 385.8 00:00:02 385.7 00:00:04 385.4 00:00:05 385.5 00:00:06 385.8 00:00:07 385.3 00:00:08 11.2 385.3 00:00:09 13.4 386.0 00:00:10 15.7 386.8 00:00:11 62.8 385.0 00:00:29 65.8 384.7 00:00:30 68.7 383.7 00:00:31 71.6 383.9...
  • Page 17 INSTRUCTION MANUAL HI 904 KARL FISCHER COULOMETRIC TITRATOR Revision 1.00 www.hannainst.com...
  • Page 18 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 19 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 21: Chapter 1. Introduction

    INTRODUCTION INTRODUCTION The HI 904 is an automatic coulometric Karl Fischer titrator with high accuracy, great flexibility and repeatability. The titrator is designed to perform titrations for a variety of applications. The main attributes of this titrator are: Flexibility Support up to 100 titration methods (standard and user defined).
  • Page 22 INTRODUCTION...

  • Page 23: Setup

    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 24: Setup

    SETUP...

  • Page 25: Unpacking

    SETUP SETUP Unpacking The titrator and the accessories are shipped in a single box containing: ITEM QUANTITY Titrator ..............1 pc. Air Pump Assembly ..........1 pc. Titration Vessel Assembly ......... 1 pc. • Glass Vessel • Accessory Port Stopper •...

  • Page 26: Safety Measures

    SETUP 14 Power Adapter ............1 pc. 15 USB Cable ............... 1 pc. 16 Instruction Manual Binder ......... 1 pc. 17 USB Storage Device ..........1 pc. 18 HI 900 PC Application (Install Kit on USB Stick) ..1 pc. 19 Quality Certificate ............

  • Page 27: Installation

    SETUP Installation 2.3.1 Titrator Top View...

  • Page 28: Titrator Rear View

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

  • Page 29: 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 Air Pump The diaphragm air pump system is designed to work with the specially designed bottle top assemblies. It allows the reagent in the titration vessel to be removed and/or replaced with minimal exposure of the interior of the vessel to ambient moisture from atmospheric humidity.

  • Page 30: Connecting The Reagent Adapter Holder

    SETUP 2.3.4.2 Connecting the Reagent Adapter Holder The Reagent Adapter Holder is a convenient dock for the Reagent Exchange Adapter when it is not in use. The holder consists of a base that fastens to the titrator pump bay and a removable standard-taper glass tube.

  • Page 31: Titration Vessel

    The titration takes place in a sealed titration vessel. The titration vessel can also be referred to as a reaction vessel, titration cell or reaction cell. The primary design features of the HI 904 titration vessel include the following: • Durability, easy to use, clean and maintain.

  • Page 32: Titration Vessel Components

    The Karl Fischer generator electrode (D) consists of two platinum electrodes (anode and cathode) on a glass body. The anode and cathode may be separated by a diaphragm that is built into the body of the generator. The HI 904 can be used with both diaphragm and diaphragm-less generators.
  • Page 33 SETUP Reagent Exchange Port The HI 904 titration vessel can be connected to the reagent and waste bottles using the Reagent Exchange port and the supplied adapter. The Reagent Exchange Adapter may remain connected to the titration vessel during operation if lower drift is not necessary. Otherwise, place the supplied glass stopper (G) in the Reagent Exchange Port.

  • Page 34: Electrical Connections

    SETUP 2.3.4.4 Electrical Connections • Connect the KF generator electrode to the 5-pin connector (C) using the supplied cable. • Connect the KF detector electrode to the BNC connector (D). • Connect the power adapter cable to the power input connector (B). Figure 5 Function Type of Connector...

  • Page 35: Reagent, Waste Bottle Assembly

    SETUP 2.3.5 Reagent, Waste Bottle Assembly The bottle top assemblies are equipped with desiccant cartridges containing molecular sieves, which ensures that the air passing through the reagent handling system has been dried. The molecular sieves have a limited capacity to absorb moisture and is typically exhausted after 3 to 5 weeks.

  • Page 36: Reagent Exchange Adapter

    SETUP 2.3.6 Reagent Exchange Adapter The Reagent Exchange Adapter is used to connect reagent and waste bottles to the titration vessel. The adapter consists of a set of o-rings and compression caps that form a seal around the reagent and waste tubes, and a ground-glass joint for connection to the titration vessel. The compression caps can be loosened when inserting tubes or adjusting the tube position and tightened to hold the tubes in place.
  • Page 37 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 38: User Interface

    USER INTERFACE...

  • Page 39: 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 a power outlet with the supplied power adapter. • Turn on the titrator using the power switch located on the back of the instrument. •...

  • Page 40: Description

    USER INTERFACE 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. Some of the keys are only active in specific screens: Starts or stops titration sequence Turns the stirrer ON and OFF ( Idle mode only)

  • Page 41: 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 42: 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 43: 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 44: 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 Options 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 45: 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...
  • Page 46 USER INTERFACE 3-10...
  • Page 47 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 Reagent Exchange Reminder .............

  • Page 48: General Options

    GENERAL OPTIONS...

  • Page 49: 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 50: 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 51: 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 52: Language

    Coulometric Karl Fischer reagents have a limited titration capacity, meaning that there is a limited amount of water that a volume of reagent can react. For this reason, the HI 904 automatically tracks the total amount of water that has been reacted since the reagent was added to the titration vessel.

  • Page 53: Save Files To Usb Storage Device

    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 904 folder, as follows: - Methods: USB Drive: \ HI 904 \ Methods \ *.mtd...

  • Page 54: 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 904 \ Methods \ *.mtd - Reports: USB: \ Drive \ HI 904 \ Reports \ *.rpt...

  • Page 55: Usb Link With Pc

    GENERAL OPTIONS 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 HI 900 PC Application installed. The titrator automatically attempts to connect to the PC while on this screen.

  • Page 56: Setup Balance Interface

    GENERAL OPTIONS Disconnect the KF electrode, then connect the HI 900940 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 57: 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 58: Reset To Default Settings

    GENERAL OPTIONS 4.13 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. 4.14 Update Software This screen allows the user to update the titrator software from a USB storage device...
  • Page 59 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 60 METHODS 5.5.10 Control Parameters ................... 5 - 16 5.5.10.1 Titration Speed .....................5 - 16 5.5.10.2 Standby Mode ....................5 - 17 5.5.10.3 Standby Duration ..................5 - 17 5.5.10.4 Imposed Current ..................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 ...................

  • Page 61: 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 HI 900 PC application or a USB storage device.

  • Page 62: 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 Options section).

  • Page 63: 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 64: Chapter 5. 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 65: Method Options

    METHODS Save method: and select Save Method to keep the changes. After making modifications, press 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 66: 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 KF Coulometric or Bromine Index.

  • Page 67: Pre-Analysis Stir Time

    METHODS 5.5.4 Pre-Analysis Stir Time To avoid erroneous results or unreachable endpoints when analyzing samples with limited solubility, the sample must be completely dissolved in the solvent prior to the start of a titration. The pre-analysis stir time can be set between 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.

  • Page 68: Stirbar Type

    METHODS 5.5.6 Stirbar Type Allows the user to edit the stirbar description. 5.5.7 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).

  • Page 69: Reagent Name

    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 name. 5-11...

  • Page 70: Sample Parameters

    METHODS 5.5.9 Sample Parameters This screen allows the user to access and configure the specific sample parameters. 5.5.9.1 Sample Determination This screen allows the user to select the sample determination mode. Normal sample determination is performed through direct titration of liquid samples that are soluble in solvent and have homogeneous distribution in water.

  • Page 71: Sample Name

    METHODS 5.5.9.2 Sample Name This screen allows the user to enter a name for the sample (up to 14 characters). Use the arrow keys 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 sample: mass or volume.

  • Page 72: Sample Size

    METHODS 5.5.9.4 Sample Size This option allows the user to enter the sample size. For External/Dissolution, enter the size of the aliquot taken from the external vessel. Before the titration is started, the user is asked again to enter the sample size. The sample size (mass or volume) can be automatically acquired from the balance (when the balance feature is enabled - see Section 4.11, Setup Balance Interface ) Sample Density ( Sample Type: Volume only)

  • Page 73: External Solvent Size

    METHODS 5.5.9.6 External Solvent Size ( External Dissolution/Extraction determination mode 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.

  • Page 74: Control Parameters

    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. 5-16...

  • Page 75: Standby Mode

    METHODS 5.5.10.2 Standby Mode When enabling this option, the titrator will automatically revert to Standby mode after a titration is completed. See also the Standby Duration option. 5.5.10.3 Standby Duration The user can enter the period of time which the cell is kept dry and ready for subsequent analysis after a titration has finished.

  • Page 76: Imposed Current

    METHODS 5.5.10.4 Imposed Current The HI 904 uses a bivoltametric indicating electrode system. During a titration, the titrator monitors the voltage required to maintain a constant polarization current (imposed current). This option allows the user to select the electrode polarization current from the predefined list.

  • Page 77: Generator Current Mode

    METHODS 5.5.10.6 Generator Current Mode This option allows the user to select the generator electrode current mode: Auto: The titrator will dynamically select the optimal current level (50-400 mA) depending on the dose size and the electrical resistance of the reagent. Fixed (400 mA): The titrator will always use 400-mA pulses.

  • Page 78: Termination Parameters

    METHODS 5.5.11 Termination Parameters This screen allows the user to set the control parameters related to the end of the titration. 5.5.11.1 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.

  • Page 79: Maximum Titrated Water

    METHODS 5.5.11.2 Maximum Water Titrated The maximum water reacted during the titration must be set according to the analysis. If the titration end point is not reached, the titration will be terminated after the maximum titrated water has been reacted. The error message (“Limits Exceeded”) will appear on the display.

  • Page 80: End Point Stability Time

    METHODS 5.5.11.4 End Point Stability Time This screen allows users to set the time period in which the electrode potential must remain stable. This setting is in accordance with the mV End Point termination criterion. 5.5.12 Result Unit The titrator provides the results based on the selected units. Printing To print method parameters, press from the main screen, then...

  • Page 81: Bromine Index

    100 g of sample. Bromine Index is expressed as mg Br/100g; Bromine Number is expressed as g Br/100g. The HI 904 can be set up to perform Bromine Index determinations by following the steps: (1)Prepare the titrator according to Section 2 of the manual, except remove all desiccant from the desiccant cartridges.
  • Page 82 METHODS 5-24...
  • Page 83 TITRATION Chapter 6. Contents TITRATION ................... 6 - 3 Idle ......................6 - 3 Pre-titration..................6 - 3 Drift Analysis ..................6 - 4 Standby ....................6 - 5 Sample Analysis ..................6 - 6...
  • Page 84 TITRATION...

  • Page 85: Chapter 6. Titration

    TITRATION Idle The titrator first enters Idle mode when it is switched on. All of the HI 904’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, software upgrades, options for interface with PC and accessories as well as burette options.

  • Page 86: Drift Analysis

    ‘dryness’ of the reagent over the course of a minute. The rate at which water leaks into the cell is then calculated and reported by the HI 904 in units of µg/min. The HI 904 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 87: Standby

    TITRATION Standby After the drift rate has been determined, the HI 904 moves into Standby mode. In standby mode, the dryness of the titration vessel is maintained and the drift rate is continuously moni- tored and updated. From Standby mode, a sample analysis, or drift rate logging session can be launched as well as method selection, customization of method parameters, and general options (exter- nal keyboard only, by pressing <<Home>>).

  • Page 88: Sample Analysis

    TITRATION 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 89 TITRATION Manual Entry Follow the steps below: 1. Attach a long needle (approximately 6 in. for best control) to a syringe that is large enough to hold at least one complete sample volume. For the volumetric addition of samples, use a precision-volume syringe. 2.
  • Page 90 TITRATION Automatic Mass Acquisition from Analytical Balance The sample size can be automatically acquired from the balance when connected to the titrator using the RS232 interface. Note: The user must make sure that the balance and the titrator are properly configured and the balance feature is enabled (see Section 4.11, Setup Balance Interface).
  • Page 91 TITRATION 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 92 TITRATION Viewing the Titration Curve During a titration, the titration curve can be displayed on the Titration Graph screen, by pressing . The titration report ID is also displayed inside the graph window. Press to stop the titration manually and return to Idle mode. Press to stop the titration and return to Standby mode.
  • Page 93 TITRATION Averaging Sample Analysis Results , the Sample Analysis History, Averaging and Statistical Data can be By pressing viewed. Use the keys to scroll the results list. to choose the results that will be used for averaging. Note: When there are no results selected, dashes will appear in the Average Sample Concentration and the Standard Deviation fields.
  • Page 94 TITRATION 6-12...

  • Page 95: Auxiliary Functions

    AUXILIARY FUNCTIONS Chapter 7. Contents AUXILIARY FUNCTIONS ............... 7 - 3 Air Pump ....................7 - 3 7.1.1 Filling the Vessel ..................7 - 3 7.1.2 Emptying the Vessel ..................7 - 3 Stirrer....................7 - 4 Results ....................7 - 4 7.3.1 Review Last Titration Report ................
  • Page 96 AUXILIARY FUNCTIONS...

  • Page 97: Chapter 7. Auxiliary Functions

    AUXILIARY FUNCTIONS AUXILIARY FUNCTIONS Air Pump The air pump is used to add or remove the reagent in the titration vessel without exposure to atmospheric moisture. To start the air pump, press from the Idle screen. The air pump can be stopped by pressing 7.1.1 Filling the Vessel To add reagent to the titration vessel:...

  • Page 98: Stirrer

    AUXILIARY FUNCTIONS Stirrer Note: When custom stirrer is selected (see Section 4.4, Stirrer in General Options chapter), the commands related to the stirrer are not available. while in Idle mode. The stirrer can be turned on and off by pressing During the titration process the stirrer cannot be turned off.

  • Page 99: Results

    AUXILIARY FUNCTIONS Results To access the “Data Parameters” screen, press button. From the Data Parameters screen you can 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 Report screen.

  • Page 100: Review Available Reports

    AUXILIARY FUNCTIONS 7.3.2 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 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 101: Meter Information

    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 102: Setup Titration Report

    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 MAINTENANCE, PERIPHERALS Chapter 8. Contents MAINTENANCE, PERIPHERALS ............8 - 3 Generator Electrode Maintenance ............8 - 3 Detector Electrode Maintenance ............8 - 3 Reagent Adapter Holder Maintenance..........8 - 4 Reagent Exchange Adapter Maintenance ..........8 - 4 Peripherals....................

  • Page 104: Maintenance, Peripherals

    MAINTENANCE, PERIPHERALS...

  • Page 105: Generator Electrode Maintenance

    MAINTENANCE, PERIPHERALS MAINTENANCE, PERIPHERALS Generator Electrode Maintenance Caution: Never heat generator electrodes over 50ºC when drying! This could cause permanent damage to the connector! Generator electrodes should be cleaned every 1-2 weeks, more frequently if working with “dirty” or “oily” samples. 1.

  • Page 106: Reagent Adapter Holder Maintenance

    MAINTENANCE, PERIPHERALS If these signs are observed, the electrode pins may be dirty. Rinse the electrode with a solvent that is appropriate for the type of sample used – methanol is usually sufficient. Remove debris by gently wiping with a clean cloth or tissue. Allow the probe to dry completely before re-installing.

  • Page 107: Peripherals

    MAINTENANCE, PERIPHERALS 5. Wipe joint grease off of the ground-glass joints with a clean, dry cloth or tissue. 6. Dry the glass adapter in a drying oven, or thoroughly wipe dry. Allow that caps and o-rings to air dry. 7. Ensure that all pieces are thoroughly dry before re-assembly. Peripherals Warning! Connection/disconnection of POWER CORD, PUMP ASSEMBLY, EXTERNAL PC DISPLAY, PRINTER, RS232 INTERFACE or EXPANSION DEVICE must be done...

  • Page 108: Connecting An External Pc Keyboard

    MAINTENANCE, 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 connector).
  • Page 109 MAINTENANCE, PERIPHERALS The correspondence between the Titrator’s Keypad and the United States 101-type external keyboar are: External PC Keyboard (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...

  • Page 110: Connecting A Printer

    MAINTENANCE, PERIPHERALS 8.5.3 Connecting a Printer A variety of parallel printers 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 printer to the standard 25–pin Socket.

  • Page 111: Connecting To A Computer

    MAINTENANCE, PERIPHERALS 8.5.4 Connecting to a Computer The titrator can be connected to a computer using a USB cable. HI 900 PC application needs to be installed on the PC. Connect the cable to the USB port on the rear panel of the titrator. Connect the cable to the USB port on the PC.
  • Page 112 MAINTENANCE, PERIPHERALS 8-10...
  • Page 113 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 Titration Speed ....................9 - 4 9.1.1.3 Signal Averaging ....................9 - 4 9.1.2 Termination Parameters ................
  • Page 114 METHODS OPTIMIZATION 9.2.5 Sample 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 Karl Fischer Reagent System..............

  • Page 115: Chapter 9. Optimization

    During a titration, no excess iodine is present. In order to maintain the set polarization current the HI 904 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 116: Titration Speed

    µg < If Automatic is selected, the HI 904 will determine the appropriate titration speed based on the estimated water content and the amount of sample added to the vessel for each titration. If over-titration frequently occurs, select a slower titration speed. If a shorter titration duration is desired, select a faster titration speed.

  • Page 117: Termination Parameters

    METHODS OPTIMIZATION 9.1.2 Termination Parameters HI 904 provides a choice of three criteria by which a titration can be considered to have reached an endpoint successfully. 9.1.2.1 Stability Time When this termination criteria is selected, a titration is considered to have reached an endpoint when the electrode potential stays below the specified endpoint potential for a period of time called the stability time.

  • Page 118: Absolute Drift Stop

    0 and 1000 seconds. 9.1.3.2 Stirring 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 is rotating at the speed set by the user.

  • Page 119: The Sample

    Determining the Optimal Sample Size The HI 904 titrates optimally in the range of 0.5 to 2.0 mg water per sample. 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.

  • Page 120: Liquid Samples

    13. Enter the calculated mass of the sample into the HI 904. 14. Start titration using the option key ‘start analysis’ from the add sample screen.

  • Page 121: Sample Preparation Techniques

    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 904 provides options for the automatic calculation of samples prepared normally, using external extraction and external dissolution. 9.2.5.1 Dilutions It is very difficult to accurately add very small amounts of sample to the titration vessel.

  • Page 122: Homogenization

    METHODS OPTIMIZATION An outline of a general procedure follows: 1. Determine the mass of an extraction bottle or flask equipped with a septum. 2. Add the extraction solvent to the bottle and determine the mass of the bottle and the solvent. In order to maximize the effectiveness of the extraction, the water content of the solvent should be as low as possible.

  • Page 123: Karl Fischer Reagent System

    METHODS OPTIMIZATION The heating temperature is sample specific and can be found in applicable standard methods. The temperatures are chosen to be as high as possible without decomposing the sample, which can result in contamination of the titration vessel. 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.
  • Page 124 METHODS OPTIMIZATION 9-12...
  • Page 125 APPENDIX 3 A3-2...
  • Page 126 MAN HI904 09/13...
  • Page 127 APPENDIX 1 Appendix 1. Contents TECHNICAL SPECIFICATIONS .............. A1-3 A1-1...
  • Page 128 APPENDIX 1 A1-2...

  • Page 129: Appendix 1. Technical Specifications

    APPENDIX 1 TECHNICAL SPECIFICATIONS Range 1 ppm to 5% Resolution 0.1 ppm %, ppm, mg/g, µg/g, mg, µg, mg/mL, µg/mL, ppt, Result Units mgBr/100g, gBr/100g, mgBr, gBr Sample Type Liquid or Solid* (external dissolution/extraction) Determination Pre-Titration Conditioning Automatic Background Drift Correction Automatic or User Selectable Value Endpoint Criteria Fixed mV persistence, Relative drift stop or Absolute drift...
  • Page 130 APPENDIX 1 Reagent Handling System Type Sealed system with integrated diaphragm air pump Desiccant Type Molecular Sieves Bottle Thread Type GL-45 Glass Connection Standard Taper 19 (using supplied adapter) Reagent/Waste Tubing PTFE Peripheral Devices Transfer methods and reports via USB connection to a PC using the HI 900 PC Software USB Flash Drive Methods and reports can be easily transferred between devices...

  • Page 131: Appendix 2. Recommended Reagents

    APPENDIX 2 Appendix 2. Recommended Reagents 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 ................. A2-3 A2-1...
  • Page 132 APPENDIX 2 A2-2...
  • Page 133 APPENDIX 2 A2 RECOMMENDED REAGENTS A2.1 Reagents for Generators with Diaphragm Sigma-Aldrich® HYDRANAL® 34836 Coulomat AG (anolyte) 34840 Coulomat CG (catholyte) General Purpose 34726 Coulomat E (anolyte) 34840 Coulomat CG (catholyte) Ethanol-based 34868 Coulomat Oil (anolyte) 34840 Coulomat CG (catholyte) Hydrocarbons/Oils 34843 Coulomat AG-H (anolyte) 34840 Coulomat CG (catholyte)
  • Page 134 APPENDIX 2 A2-4...
  • Page 135 APPENDIX 3 Appendix 3. Accessories TITRATOR COMPONENTS ..............A3-3 A3-1...
  • Page 136 APPENDIX 3 A3-2...

  • Page 137: Appendix 3. Titrator Components

    APPENDIX 3 TITRATOR COMPONENTS HI 900561 HI 900182 Titration Vessel Reagent Adapter Holder (Glass only) (Glass only) HI 76330 Detector Electrode HI 900560 Titration Vessel Assembly HI 900511 Generator Electrode with Diaphragm HI 900512 Generator Electrode without Diaphragm HI 900180 Air Pump HI 900181 Reagent Adapter...
  • Page 138 APPENDIX 3 HI 900568 HI 900564 Reagent Exchange Desiccant Cartridge for Adapter Generator Electrodes HI 900537 HI 900542 Bottle Top Assembly (with molecular sieves) O-ring set HI 900538 HI 900534 Desiccant Cartridge for Waste Bottle Reagent/Waste Bottles HI 900535 2 x Tubing for Reagent/ HI 900551 Waste Handling Molecular sieves, 150 g...
  • Page 139 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 A3-5...
  • Page 140 MAN HI904 09/13...
  • Page 141 GENERAL APPLICATIONS BROCHURE HI 904 KARL FISCHER COULOMETRIC TITRATOR www.hannainst.com...
  • Page 143 Method ID: HI9001EN Titrator Validation with 1.0 mg/g Water Standard Description: of the needle, dip the end of the needle briefly in Method for validation of titrator accuracy. the solvent. results are expressed in mg/g and shouldmatch the  Remove the needle from the titration vessel and certified value (within the uncertainty limits) provided weigh the syringe again in order to determine the by the manufacturer of the standard.
  • Page 145 Method ID: HI9301EN Moisture Determination in Solvent for external dissolution or extraction Description: needle, dip the end of the needle briefly in the Method for the determination of moisture in solvent. extraction/dissolution solvent. The results are  Remove the needle from the titration vessel and expressed in mg/g and should be less than 1.00 weigh the syringe again in order to determine the mg/g.
  • Page 147 Method ID: HI9901EN Bromine Index of Aromatic Hydrocarbons Adaptation of ASTM D1492-08 Description: titration vessel through the septum using the Method for the determination of bromine index of needle. Pay attention not to get any sample on bromine-reactive substances. This method typically the electrode or vessel walls.
  • Page 148 Method ID: HI9901EN Bromine Index of Aromatic Hydrocarbons Adaptation of ASTM D1492-08 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:ss] Generator Electrode Type: HI 900518...
  • Page 149 TITRATION THEORY TITRATION THEORY Principles HI 904 KARL FISCHER COULUMETRIC TITRATOR Revision 1.0 www.hannainst.com...
  • Page 150 TITRATION THEORY...
  • Page 151 TITRATION THEORY Contents GENERAL REVIEW OF TITRATION THEORY ..........5 1.1 Introduction to Titrations ................5 1.2 Uses of Titrations ..................5 1.3 Advantages and Disadvantages of Titrations ..........6 TYPES OF TITRATION .................. 7 2.1 Titrations According to The Measurement Method ........7 2.1.1 Amperometric Titrations ..................
  • Page 152 TITRATION THEORY 4.3.2.2 Dispensing Errors....................22 4.3.3 Chemical Reaction Errors ................22 4.3.4 End Point Determination Errors ...............22 CALCULATIONS ..................23 5.1 Equations Used in Karl Fischer Titrations ..........23 5.1.1 Calculation of water content as % mass from samples measured by mass ..23 5.1.2 Calculation of water content as % mass from samples measured by volume ..

  • Page 153: Introduction

    TITRATION THEORY GENERAL REVIEW OF TITRATION THEORY 1.1 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 154: Advantages And Disadvantages Of Titrations

    TITRATION THEORY 1.3 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 155: Types Of Titration

    TITRATION THEORY TYPES OF TITRATIONS 2.1 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 156: Spectrophotometric Titrations

    TITRATION THEORY 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. The potential that develops in the electrochemical cell is the result of the free energy change that would occur if the chemical phenomena were to proceed until the equilibrium condition has been satisfied.

  • Page 157: Titrations According To The Reaction Type

    TITRATION THEORY 2.2 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 158: Volumetric 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 159: Generator Electrodes With Diaphragm

    TITRATION THEORY The amount of current that passes through the generator can easily and accurately be measured by the electronics of the titrator. Therefore, coulometric Karl Fischer titrations are considered absolute - standardization is not necessary. Water standards can be titrated as a system check to ensure proper system functioning.

  • Page 160: Visual Indication Of Karl Fisher Titrations

    TITRATION THEORY 2.2.1.4 Visual Indication of Karl Fischer Titrations Visual methods, originally used by Karl Fischer, are limited in application, require a high degree of skill and have been made obsolete by electrometric indication. For successful visual indication, titration samples must be colorless. Additionally, the solution coloration varies between polar and non-polar titration media.

  • Page 161: 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 ) is applied between the electrode pins or rings and the resulting voltage is measured in order to monitor the titration progress.

  • Page 162: 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 163: Complexometric Titrations

    TITRATION THEORY 2.2.4 Complexometric Titrations A complex is a species where a central metal ion is covalently bonded to one or more electron donating groups called ligands. In a complexometric titration, metal ions are titrated using a titrant that binds strongly to it. Often these titrants contain EDTA or CDTA, polydentate ligands that form very stable coordination compounds with metal ions.

  • Page 164: Precipitation Titrations

    TITRATION THEORY Titration of Acids Weak acids with pK ’s up to about 11 can be titrated in non-aqueous solvents. These include carboxylic acids, enols, phenols, imides, sulfonic acids, and inorganic acids. Water or lower alcohols are suitable for titrating medium to strong acids (pK less than 5).

  • Page 165: Titrations According To The Titration Sequence

    TITRATION THEORY Figure 6. Figure 7. 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 166 TITRATION THEORY Figure 8.

  • Page 167: Introduction To Titration Apparatus And Typical Titration Procedure

    TITRATION THEORY INTRODUCTION TO TITRATION APPARATUS AND TYPICAL TITRATION PROCEDURE 3.1 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 168: Automatic Titration

    TITRATION THEORY 3.2 Automatic Titration Automatic titrators are high-precision analytical instruments that deliver the titrant, monitor the physical change associated with the titration reaction, automatically stops at the endpoint and calculates the concentration of the analyte. Automatic titrators are best for repetitive titrations and high-accuracy analyses.

  • Page 169: Titration Results

    TITRATION THEORY TITRATION RESULTS 4.1 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. 4.2 Repeatability Repeatability, or the agreement between replicate determinations, is expressed quantitatively as the relative standard deviation (RSD).

  • Page 170: 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 171: Calculations

    TITRATION THEORY CALCULATIONS 5.1 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)

  • Page 172: Calculation Of Water Content In External Dissolution 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 173: 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) 5.2 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 174: 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 175: 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 176: 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. Electrodes respond to activity.
  • Page 177 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 equivalence 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 178 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 179 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 180 TITRATION THEORY...

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