Hanna-instruments HI 904 Instrukcja Użytkownika

1QUICK START GUIDEHI 904KARL FISCHERCOULOMETRIC TITRATORRevision 1.0www.hannainst.com

10QUICK START GUIDEBEFORE PERFORMING THE FIRST TITRATIONSetup the Titrator• Make sure that all of the titrator assemblies are properly installed (see

7-6AUXILIARY FUNCTIONS7.3.2 Review Available ReportsUp to 100 reports can be saved on the titrator. To view one of the saved reports highlight areport

7-7AUXILIARY FUNCTIONSCompany Name:Allows the company name to be recorded in each report.Operator Name:Allows the operator name to be recorded in each

7-8AUXILIARY FUNCTIONS7.3.5 Setup Titration ReportCustomize a unique report to record the titration results. An asterisk means that it will beincluded

8-1MAINTENANCE, PERIPHERALSChapter 8. Contents8 MAINTENANCE, PERIPHERALS ... 8-38.1 Generato

8-2MAINTENANCE, PERIPHERALS

8-3MAINTENANCE, PERIPHERALS8 MAINTENANCE, PERIPHERALS8.1 Generator Electrode MaintenanceCaution: Never heat generator electrodes over 50ºC when drying

8-4MAINTENANCE, PERIPHERALSIf these signs are observed, the electrode pins may be dirty. Rinse the electrode with asolvent that is appropriate for the

8-5MAINTENANCE, PERIPHERALS5. Wipe joint grease off of the ground-glass joints with a clean, dry cloth or tissue.6. Dry the glass adapter in a drying

8-6MAINTENANCE, PERIPHERALS8.5.2 Connecting an External PC KeyboardThis connection allows you to use an external PS/2 PC Keyboard in addition to titra

8-7MAINTENANCE, PERIPHERALSThe correspondence between the Titrator’s Keypad and the United States 101-type externalkeyboar are:External PC Keyboard(Un

11QUICK START GUIDEFill Titration Vessel with ReagentThe titration vessel must be filled with reagent up to the MIN marker (about 75 mL):• Lower the r

8-8MAINTENANCE, PERIPHERALS8.5.3 Connecting a PrinterA variety of parallel printers can be connected to the parallel port of the titrator using astand

8-9MAINTENANCE, PERIPHERALS8.5.4 Connecting to a ComputerThe titrator can be connected to a computer using a USB cable. HI 900 PC applicationneeds to

8-10MAINTENANCE, PERIPHERALS

9-1METHODS OPTIMIZATIONChapter 9. Contents9 OPTIMIZATION ... 9-39.1

9-2METHODS OPTIMIZATION9.2.5 Sample Preparation Techniques ... 9-99.2.5.1 Dilutions ..

9-3METHODS OPTIMIZATION9 OPTIMIZATION9.1 Titration SettingsThis section provides the descriptions of critical titration parameters necessary for an an

9-4METHODS OPTIMIZATIONnoitaziraloPtnerruC1 ΑµΑµ2 Αµ5 Αµ01tniopdnElaitnetoPVm09ot03 Vm031ot09 Vm081ot041 Vm003ot002The table that follows correlates e

9-5METHODS OPTIMIZATION9.1.2 Termination ParametersHI 904 provides a choice of three criteria by which a titration can be considered to havereached an

9-6METHODS OPTIMIZATION9.1.2.2.2 Absolute Drift StopUnder this criteria, a titration reaches an endpoint successfully when the drift falls below apred

9-7METHODS OPTIMIZATION9.2 The Sample9.2.1 Proper Sampling ProcedureProper sampling is essential for accurately determining the water content of bulk

12QUICK START GUIDELiquid Samples:• Samples with low viscosity will be added using a syringe with needle (injectionthrough the septum).• Weigh the syr

9-8METHODS OPTIMIZATION9.2.4 Liquid SamplesThe water contained in liquid samples must be available to react with the KF reagent. It isimportant to sel

9-9METHODS OPTIMIZATION9.2.5 Sample Preparation TechniquesWhile many samples can be introduced directly into the titration vessel (see section 6.5Samp

9-10METHODS OPTIMIZATIONAn outline of a general procedure follows:1. Determine the mass of an extraction bottle or flask equipped with a septum.2. Add

9-11METHODS OPTIMIZATIONThe heating temperature is sample specific and can be found in applicable standard methods.The temperatures are chosen to be a

9-12METHODS OPTIMIZATION

A3-2APPENDIX 3

A3-6APPENDIX 3MAN HI904 09/13

A1-1APPENDIX 1Appendix 1. ContentsA1 TECHNICAL SPECIFICATIONS ... A1-3

A1-2APPENDIX 1

A1-3APPENDIX 1A1 TECHNICAL SPECIFICATIONSRange 1 ppm to 5%Resolution 0.1 ppmResult Units %, ppm, mg/g, µg/g, mg, µg, mg/mL, µg/mL, ppt,mgBr/100g, gBr/

13QUICK START GUIDEUnderstanding the Displayed InformationDuring a titration, the following screen is displayed:Viewing Graph During TitrationPress

A1-4APPENDIX 1Reagent Handling SystemType Sealed system with integrated diaphragm air pumpDesiccant Type Molecular SievesBottle Thread Type GL-45Glass

A2-1APPENDIX 2Appendix 2. Recommended ReagentsA2 RECOMMENDED REAGENTS ... A2-3A2.1 Reage

A2-2APPENDIX 2

A2-3APPENDIX 2A2 RECOMMENDED REAGENTSA2.1 Reagents for Generators with DiaphragmSigma-Aldrich® HYDRANAL®34836 Coulomat AG (anolyte) 34840 Coulomat CG

A2-4APPENDIX 2

A3-1APPENDIX 3Appendix 3. AccessoriesA3 TITRATOR COMPONENTS ... A3-3

A3-2APPENDIX 3

A3-3APPENDIX 3HI 900561Titration Vessel(Glass only)HI 76330Detector ElectrodeHI 900511Generator Electrodewith DiaphragmHI 900512Generator Electrodewit

A3-4APPENDIX 3HI 900568Reagent ExchangeAdapterHI 900537Bottle Top Assembly(with molecular sieves)HI 900538Desiccant Cartridge forReagent/Waste Bottles

A3-5APPENDIX 3HI 900804Manual (English) forHI 904HI 900900UPC Application on USBFlash DriveHI 920013USB CableHI 900567Septum Kit (5 pcs)HI 900543Glass

14QUICK START GUIDE• The Review Result screen will be displayed.• Use the and keys to display information related to the last titration performed.

A3-6APPENDIX 3MAN HI904 09/13

1GENERAL APPLICATIONS BROCHUREHI 904KARL FISCHERCOULOMETRIC TITRATORwww.hannainst.com

Method ID: HI9001ENTitrator Validation with 1.0 mg/g Water StandardTitrator Application Methods: General Applications – r. 1.0Description:Method for

Method ID: HI9301ENMoisture Determination in Solventfor external dissolution or extractionTitrator Application Methods: General Applications – r. 1.0D

Method ID: HI9901ENBromine Index of Aromatic HydrocarbonsAdaptation of ASTM D1492-08Titrator Application Methods: General Applications – r. 1.0Descrip

Method ID: HI9901ENBromine Index of Aromatic HydrocarbonsAdaptation of ASTM D1492-08Titrator Application Methods: General Applications – r. 1.0Results

1TITRATION THEORYTITRATION THEORYPrinciplesHI 904KARL FISCHERCOULUMETRIC TITRATORRevision 1.0www.hannainst.com

15QUICK START GUIDE• Transferring a report file will automatically transfer the corresponding log file andtitration graph BMP file (if applicable).• P

2TITRATION THEORY

3TITRATION THEORYContents1 GENERAL REVIEW OF TITRATION THEORY ... 51.1 Introduction to Titrations ...

4TITRATION THEORY4.3.2.2 Dispensing Errors... 224.3.3 Chem

5TITRATION THEORY1 GENERAL REVIEW OF TITRATION THEORY1.1 Introduction to TitrationsA titration is a quantitative, volumetric procedure used in analyti

6TITRATION THEORY1.3 Advantages and Disadvantages of TitrationsSome advantages of titrations, as an analytical technique, are:• More precise results t

7TITRATION THEORYFigure 1.2 TYPES OF TITRATIONS2.1 Titrations According to The Measurement Method2.1.1 Amperometric TitrationsAn amperometric titratio

8TITRATION THEORYPotentiometry is the measurement of a potential under conditions of zero current flow. Themeasured potential can then be used to dete

9TITRATION THEORY2.2 Titrations According to The Reaction Type2.2.1 Karl Fischer TitrationsThis method is based on a well-defined chemical reaction be

10TITRATION THEORYof reaction decreases and titration endpoint become increasingly difficult to reach. If the pHexceeds 8, side reactions begin to occ

11TITRATION THEORYThe amount of current that passes through the generator can easily and accurately be measuredby the electronics of the titrator. The

16QUICK START GUIDEQS 90408/13 Nr Titr Water[µg] mV Time 0 0.0 385.7 00:00:00 1 0.0 385.7 00:00:01 2

12TITRATION THEORY2.2.1.4 Visual Indication of Karl Fischer TitrationsVisual methods, originally used by Karl Fischer, are limited in application, req

13TITRATION THEORY1502002503003504004500 0.2 0.4 0.6 0.8 1Potential (mV)Titrant Volume (mL)Karl Fischer Titration, Bivoltametric Indication vs. Titran

14TITRATION THEORYpClFigure 3.Figure 4.Figure 3 shows a traditional titration curve. The curve is obtained by plotting the pH valueagainst the volume

15TITRATION THEORYFigure 5.2.2.4 Complexometric TitrationsA complex is a species where a central metal ion is covalently bonded to one or moreelectron

16TITRATION THEORYTitration of AcidsWeak acids with pKa’s up to about 11 can be titrated in non-aqueous solvents. These includecarboxylic acids, enols

17TITRATION THEORYFigure 7.Figure 6.Visual indicators such as Ferrion are also available. The oxidized and reduced form of theindicator will have diff

18TITRATION THEORYABFigure 8.Potential, glass electrode, mVC

19TITRATION THEORY3 INTRODUCTION TO TITRATION APPARATUS AND TYPICALTITRATION PROCEDURE3.1 Manual TitrationApparatus required for manual titration incl

20TITRATION THEORY3.2 Automatic TitrationAutomatic titrators are high-precision analytical instruments that deliver the titrant, monitorthe physical c

21TITRATION THEORY4 TITRATION RESULTS4.1 AccuracyThe factors most critical to achieving accurate results with the HI 900 titration systems arethe conc

1INSTRUCTION MANUALHI 904KARL FISCHERCOULOMETRIC TITRATORRevision 1.00www.hannainst.com

22TITRATION THEORY4.3.2.2 Dispensing ErrorsIncorrect dispensing due to:• Dead valve volume and leaking valve;• Inaccuracy in motor drive and gear lash

23TITRATION THEORY       

24TITRATION THEORY    

25TITRATION THEORY        

26TITRATION THEORY       

27TITRATION THEORY  

28TITRATION THEORY6 GLOSSARYAcidA chemical species that can donate one or more protons (hydrogen ions).Acid-Base TitrationStoichiometric neutralizatio

29TITRATION THEORYEnd pointThe point where a titration is stopped because a physical change in the solution hasindicated a completed titration. Titrat

30TITRATION THEORYNeutralizationA chemical reaction where an acid and a base react to form a neutral salt and water.Non-aqueousA solution that does no

31TITRATION THEORYSpectrophotometric TitrationA titration in which the end point is marked by a change in the color and/or colorintensity.Stoichiometr

2Dear customer,Congratulations on choosing a Hanna Instruments product.Please read this instruction manual carefully before using the instrument. This

32TITRATION THEORYTitr THEORY 90407/13

3TABLE OF CONTENTSChapter 1. INTRODUCTIONChapter 2. SETUPChapter 3. USER INTERFACEChapter 4. GENERAL OPTIONSChapter 5. METHODSChapter 6. TITRATIONChap

2QUICK START GUIDEDear customer,Congratulations on choosing a Hanna Instruments Product.This guide has been written for the HI 904 Karl Fischer Coulom

4

1-1INTRODUCTION1 INTRODUCTIONThe HI 904 is an automatic coulometric Karl Fischer titrator with high accuracy, great flexibilityand repeatability.The t

1-2INTRODUCTION

2-1SETUPChapter 2. Contents2 SETUP ... 2-32.1 Unpacki

2-2SETUP

2-3SETUP2 SETUP2.1 UnpackingThe titrator and the accessories are shipped in a single box containing:ITEM QUANTITY1 Titrator ...

2-4SETUP14 Power Adapter ... 1 pc.15 USB Cable ...

2-5SETUP2.3 Installation2.3.1 Titrator Top View

2-6SETUP2.3.2 Titrator Rear View2.3.3 Titrator Left-side View

2-7SETUP2.3.4 Titrator AssemblyNote: Assembly operations must be completed before connecting the titrator to the power supply!2.3.4.1 Connecting the A

3QUICK START GUIDEContentsINTRODUCTION ...5SAFE

2-8SETUP2.3.4.2 Connecting the Reagent Adapter HolderThe Reagent Adapter Holder is a convenient dock for the Reagent Exchange Adapter when itis not i

2-9SETUPFigure 32.3.4.3 Titration VesselThe titration takes place in a sealed titration vessel. The titration vessel can also be referredto as a react

2-10SETUP2.3.4.3.1 Titration Vessel ComponentsWarning: Always apply a thin layer of joint grease (supplied) to ground-glass joints beforeattaching. I

2-11SETUP Reagent Exchange PortThe HI 904 titration vessel can be connected to the reagent and waste bottles using theReagent Exchange port and the su

2-12SETUP2.3.4.4 Electrical Connections• Connect the KF generator electrode to the 5-pin connector (C) using the supplied cable.• Connect the KF detec

2-13SETUP2.3.5 Reagent, Waste Bottle AssemblyThe bottle top assemblies are equipped with desiccant cartridges containing molecular sieves,which ensure

2-14SETUP2.3.6 Reagent Exchange AdapterThe Reagent Exchange Adapter is used to connect reagent and waste bottles to the titrationvessel. The adapter c

3-1USER INTERFACEChapter 3. Contents3 USER INTERFACE... 3-33.1 Start U

3-2USER INTERFACE

3-3USER INTERFACE3 USER INTERFACE3.1 Start UpOnce the instrument is assembled and installed, follow the steps below to start the titrator:• Connect th

4QUICK START GUIDE

3-4USER INTERFACE3.2 DescriptionThis chapter describes the basic principles of navigation through the user interface, selectingfields and entering val

3-5USER INTERFACE3.2.1.3 Arrow KeysThese keys have the following functions:• Move the on-screen cursor.• Increase and decrease the stirrer speed and o

3-6USER INTERFACE3.2.3 The Idle ScreenAfter start up and initialization, the first screen displayed is the Idle Screen.Idle Screen fields:Method name:

3-7USER INTERFACE3.2.4 The Process ScreenWhen the user presses while in Idle Screen, all titration related processes are started.The titrator displa

3-8USER INTERFACE3.3.1 Selecting an OptionTo select an option, simply press the option key below thevirtual key. For example, to access the Method Opt

3-9USER INTERFACE3.3.4 Saving ModificationsThe Saving Method screen allows the user to save themodifications. To exit from Saving Method screen withou

3-10USER INTERFACE

4-1GENERAL OPTIONSChapter 4. Contents4 GENERAL OPTIONS ... 4-34.1 Date and

4-2GENERAL OPTIONS

4-3GENERAL OPTIONS4 GENERAL OPTIONSThe General Options screen gives access to options that are not directly related to thetitration process. To access

5QUICK START GUIDEINTRODUCTIONThe HI 904 Karl Fischer Coulometric titrator is extremely flexible, capable of performing awide variety of highly accura

4-4GENERAL OPTIONS4.2 Display SettingsThis screen allows the user to customize the viewing features of the display.Option Keys:Increases the backlight

4-5GENERAL OPTIONS4.3 BeeperThis screen allows the user to turn the Beeper On (Enable) or Off (Disable).The beeper will sound after a titration is com

4-6GENERAL OPTIONS4.5 LanguageSelect an available language.4.6 Reagent Exchange ReminderCoulometric Karl Fischer reagents have a limited titration ca

4-7GENERAL OPTIONS4.7 Save Files to USB Storage DeviceThis option allows the user to save files from titrator to a USB storage device.On the titrator,

4-8GENERAL OPTIONS4.8 Restore Files from USB Storage DeviceThis screen allows the user to transfer files from the USB storage device to the titrator.I

4-9GENERAL OPTIONS4.9 USB Link with PCThe USB Link feature is useful to transfer methods/reports directly to/from a PC. To use thisfeature, connect th

4-10GENERAL OPTIONSDisconnect the KF electrode, then connect the HI 900940 calibration key to the electrodeinput (BNC connector).Depending on which pa

4-11GENERAL OPTIONSConfigure the settings on the titrator Balance Configuration menu to match the settings foryour particular balance (baud rate, data

4-12GENERAL OPTIONS4.13 Reset to Default SettingsThis option restores the manufacturer settings.Note: Please be careful!!! This will also delete all t

5-1METHODSChapter 5. Contents5 METHODS ... 5 - 35.1 Select

6QUICK START GUIDESAFETY MEASURESThe following safety measures must be followed:1. Never connect or disconnect the pump assemblies with the titrator t

5-2METHODS5.5.10 Control Parameters ... 5 - 165.5.10.1 Titration Speed

5-3METHODS5 METHODSAll of the parameters required to complete an analysis are grouped into a method.The titrator is supplied with a pack of standard m

5-4METHODS5.2 Standard MethodsThe standard methods were developed for the most common types of analysis. Also, thestandard methods can be used as a mo

5-5METHODS5.2.3 Restoring the Standard Methods to the Manufacturer SettingsYou can restore the standard method to the manufacturer setting by highligh

5-6METHODSNote: Only a limited number of user methods can be generated. The titrator can hold 100methods (standard and user). When it is reached, a wa

5-7METHODSSave method:After making modifications, press and select Save Method to keep the changes.5.5 Method Options5.5.1 Naming the User MethodTh

5-8METHODS5.5.2 Method RevisionThis option allows you to enter a string representing the current method revision. Therevision string format should be

5-9METHODS5.5.4 Pre-Analysis Stir TimeTo avoid erroneous results or unreachable endpoints when analyzing samples with limitedsolubility, the sample mu

5-10METHODS5.5.6 Stirbar TypeAllows the user to edit the stirbar description.5.5.7 Drift EntryAllows the user to choose the drift entry mode that is u

5-11METHODS5.5.8 ReagentThe user can enter a name for the reagent (up to 15 characters). Use the arrow keys tonavigate through the character table; pr

7QUICK START GUIDETITRATOR CONNECTIONSFront ViewRear View

5-12METHODS5.5.9 Sample ParametersThis screen allows the user to access and configure the specific sample parameters.5.5.9.1 Sample DeterminationThis

5-13METHODS5.5.9.2 Sample NameThis screen allows the user to enter a name for the sample (up to 14 characters). Use thearrow keys to navigate through

5-14METHODS5.5.9.4 Sample SizeThis option allows the user to enter the sample size. For External/Dissolution, enter the sizeof the aliquot taken from

5-15METHODS5.5.9.6 External Solvent Size ( External Dissolution/Extraction determination modeonly)Enter the mass of the solvent used for external diss

5-16METHODS5.5.10 Control ParametersThe user can access and edit the parameters related to the titration.5.5.10.1 Titration SpeedChoose the desired ti

5-17METHODS5.5.10.2 Standby ModeWhen enabling this option, the titrator will automatically revert to Standby mode after atitration is completed.See al

5-18METHODS5.5.10.4 Imposed CurrentThe HI 904 uses a bivoltametric indicating electrode system. During a titration, the titratormonitors the voltage r

5-19METHODS5.5.10.6 Generator Current ModeThis option allows the user to select the generator electrode current mode:Auto:The titrator will dynamicall

5-20METHODS5.5.11.1 Maximum DurationSpecify the maximum time a titration is allowed to run. Once this point is reached, thetitration will be terminate

5-21METHODS5.5.11.3 Termination CriterionThis screen allows the user to set the titration termination criterion.mV End PointThe titration is terminate

8QUICK START GUIDEUSER INTERFACEKeypadThe titrators have their own keypad with 29 keys grouped in four categories, as follows:DisplayThe titrators hav

5-22METHODS5.5.12 Result UnitThe titrator provides the results based on the selected units.5.6 PrintingTo print method parameters, press from the ma

5-23METHODS5.7 Bromine IndexThe HI 904 is capable of performing Bromine Index/Bromine Number determinations. Bro-mine Index/Number is a measure of th

5-24METHODS

6-1TITRATIONChapter 6. Contents6 TITRATION ... 6-36.1 Idle ..

6-2TITRATION

6-3TITRATION6 TITRATION6.1 IdleThe titrator first enters Idle mode when it is switched on. All of the HI 904’s software featuresand adjustable paramet

6-4TITRATIONDuring the pre-titration, the user cannot change the currently selected method or access themethod parameters.Note: If the pre-titration l

6-5TITRATION6.4 StandbyAfter the drift rate has been determined, the HI 904 moves into Standby mode. In standbymode, the dryness of the titration vess

6-6TITRATION6.5 Sample AnalysisWhile in Standby mode, press .Note: If the drift value is zero a warning message appears to inform the user that theso

6-7TITRATIONManual EntryFollow the steps below:1. Attach a long needle (approximately 6 in. for best control) to a syringe that is largeenough to hold

9QUICK START GUIDEHOW TO SELECT YOUR LANGUAGETo change the language, press from the mainscreen. Highlight the Language option and thenpress . Using

6-8TITRATIONAutomatic Mass Acquisition from Analytical BalanceThe sample size can be automatically acquired from the balance when connected to thetitr

6-9TITRATIONThe titrator returns to the previous screen and the sample size is automatically updated.Now the analysis can be started.Start AnalysisPre

6-10TITRATIONViewing the Titration CurveDuring a titration, the titration curve can be displayed on the Titration Graph screen, bypressing . The titr

6-11TITRATIONAveraging Sample Analysis ResultsBy pressing , the Sample Analysis History, Averaging and Statistical Data can beviewed.Use the and

6-12TITRATION

7-1AUXILIARY FUNCTIONSChapter 7. Contents7. AUXILIARY FUNCTIONS ... 7-37.1 Air Pu

7-2AUXILIARY FUNCTIONS

7-3AUXILIARY FUNCTIONS7 AUXILIARY FUNCTIONS7.1 Air PumpThe air pump is used to add or remove the reagent in the titration vessel without exposureto at

7-4AUXILIARY FUNCTIONS7.2 StirrerNote: When custom stirrer is selected (see Section 4.4, Stirrer in General Options chapter),the commands related to t

7-5AUXILIARY FUNCTIONS7.3 ResultsTo access the “Data Parameters” screen, press button.From the Data Parameters screen you can access the following o