51709617 01 10.12 DL5x - Mettler Toledo

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Quick GuideDL50/DL53/DL55/DL58Titrators

ContentsContentsPage1.Introduction .32.Safety measures .53.3.13.1.13.1.23.1.33.1.43.2The titrator .The operating concept .The Menu keys .The Auxiliary function keys .The Command keys .The Entry keys .Changing the language .6789910114.4.14.1.14.2How to perform your first titration .Preparations .Filling (rinsing) burette .Performing titration method 90001 .121213145.5.15.25.3The method concept .METTLER methods .Standard methods .Generating a method .192020246.6.16.2How to calibrate a pH electrode .Zero point and slope .Calibration .2626277.7.17.27.2.17.2.27.3How to determine the titer of an NaOH solution .Titer t .Preparations .Modifying a standard method .Titrant and primary standard .Determining the titer .3030303031328.How to measure the pH value of a solution .359.Storing sample data .36METTLER TOLEDO DL50/DL53/DL55/DL581

2METTLER TOLEDO DL50/DL53/DL55/DL58

Introduction1.IntroductionThe METTLER TOLEDO DL50, DL53, DL55 and DL58 Titrators are microprocessor controlled analytical instruments which supply accurate and reproducible results thanks to theirbuilt-in intelligence.You can use the titrators to perform end point, equivalence point and pH-stat titrations, tomeasure the potential and temperature of solutions, as well as to determine TAN/TBN andacid and base capacities. Voltametric and amperometric titrations can be performed using aKF option and the moisture content determined by the Karl Fischer method with a KF titrationstand. You can perform conductivity measurements and conductometric titrations with athird-party device equipped with an analog output.In addition to electrodes, temperature sensors and a stirrer, you can also attach an analogrecorder to the titrators. You can attach an external keyboard to the DIN socket whichpermits not only text entries but also remote control of the titrator. You can also connect abar-code reader to this keyboard. Maximum two TTLIO sockets are used for the attachmentof devices you can control via the inputs and outputs.With the Centronics option you can attach a balance to the RS232 interface, which transfers the sample weight automatically, and a printer, which records the desired data.With an RS option you can attach a computer, which interchanges data with the titrator, or a terminal for use as an auxiliarydisplay, and a sample changer from METTLER TOLEDO for the automatic analysis of sample series.The titrators have a slot for a memory card on which you can store your method andmeasured data. In the DL50 case, only a software update with a card is possible.While the four titrators are operated in the same manner, they differ in regard to theirhardware and software; these differences are indicated in the relevant sections.METTLER TOLEDO DL50/DL53/DL55/DL583

IntroductionWhere can I find what information?1. This Quick Guide will help you learn to operate the titrator within a short space of time.You will perform your first analyses with the aid of stored methods.2. The Reference Handbook provides a complete description of the operating principles ofthe four titrators. You will find the installation instructions in Section 10. The additionalcommands and functions, which offers the DL58, are described in Section 7. The index inSection 13 includes key words from both the Quick Guide and the Reference Handbook.3. The application brochure describes 30 METTLER methods; 4 methods are stored in theDL50, 20 in the DL53 and 30 in the DL55 and DL58.4. The Computer Interface Description, namely a detailed explanation of the communication between titrator and computer, can be ordered.4METTLER TOLEDO DL50/DL53/DL55/DL58

Safety measures2.Safety measuresThe titrators have been tested for the experiments and intended purposes documented inthe Quick Guide and the Reference Handbook. However, this does not absolve you from theresponsibility of performing your own tests of the products supplied by us regarding theirsuitability for the methods and purposes you intend to use them for. You should thereforeobserve the following safety measures.Measures for your protectionRisk of electricshock– Ensure that you plug the power cable supplied into a receptacle outlet thatis grounded! In the absence of grounding, a technical fault could be lethal.– Switch the instrument off and disconnect the power cable before you openthe housing! An electric shock could be lethal.– Never work in an environment subject to explosion hazards! The housingof the instrument is not gas tight (explosion hazard due to spark formation,corrosion caused by the ingress of gases).Risk of explosion– Always test the titration vessel for firm seating in the titration head! If it fallsoff, you could injure yourself if working with toxic titrants and solvents orstrong acids or bases.Risk of corrosion– When using chemicals and solvents, comply with the instructions of theproducer and the general lab safety rules!Measures for operational safetyCaution– Have the instrument serviced only by METTLER TOLEDO Service!– Always wipe off splashed liquids immediately! The instrument is notwater-proof.– Exclude the following environmental influences: powerful vibrations, direct sunlight, atmospheric humidity greater than 80%, temperatures below 5 C and above 40 C, powerful electric or magnetic fields!METTLER TOLEDO DL50/DL53/DL55/DL585

The titrator3.The titratorBurette at drive 2Connection socket forexternal keyboard (notvisible)Titration stand(Stand 1)Slot for memory cardRear view(the diagram refers to the standard equipment with pH and Centronicsoptions)Connections forReference electrodeElectrode (sensor)TTLIO socketTemperature sensorBalance connectionStirrerAnalog recorderPrinter connectionSocket for power cableOn/off switchYou have installed your titrator (see Section 10 of the Reference Handbook) and would liketo start titrating immediately. Before you start, however, you must be familiar above all withthe functions of the keys and be capable of following the display in the language of yourchoice: All texts in the titrator are available in English, German, French, Spanish and Italian.Note: Please leave the titrator switched on during the first 48 hours to allow the built-inbattery (rechargeable battery) to become fully charged. This battery supplies theinternal clock with power when the titrator is switched off. If the titrator is not used for4 months or more, you may well have to recharge the battery and reset the time.6METTLER TOLEDO DL50/DL53/DL55/DL58

The titrator3.1The operating conceptAfter you have switched on the titrator, it always performs a self-test before the display of thetitrator name appears (example showing DL55):Display (mask)METTLER TTOLEDOResetArrow keysDL55Version 2.xCommand keysAuxiliaryfunction SetupSampleMethodRunF4F5()789[]456123/*Entry keysMisc.*.ShiftDataTransfer0.CEDelMenu keysAll Menu and Auxiliary function keys can now be activated.– Press, e.g. the Setup key:Title rature sensorsName of thekey, i.e. thedisplayed list ofresources ispart of theSetup menu PrintModifyCommandsIn addition to the Menu and Auxiliary function keys, you can now activate the key, Resetand Command keys F3 , "Print" and F4 , "Modify". :The arrow in the display means that the list contains additional resources.When you press the key, the lines are scrolled upward, the selection bar is fixed.The commands you can execute always refer to the line that is selected.Reset: The initial mask "METTLER TOLEDO." reappears: Pressing Reset aborts analyses or other actions.METTLER TOLEDO DL50/DL53/DL55/DL587

The titratorPrint(press F3 ): The list of titrants is printed out (if a printer is attached and defined,see Section 2.7 of the Reference Handbook).Modify (press F4 ): The list of titrants appears:TitrantsNaOHHClHCl04Esc0.1 mol/L0.1 mol/L0.1 mol/LDeleteSETUP AddModifyOK– Press the Reset key to display the initial mask again.3.1.1The Menu keysFor an analysis of a sample to be performed automatically, the required data must be stored.In the titrator, these data are assigned to sets of particular operations, the menus, and can beaccessed with the Menu keys. It is the coordination between these menus that permitsautomatic analysis.SetupAll resources such as titrants and electrodes needed for the titration arestored in the Setup menu.MethodThe sample is determined using a method. All methods needed for thedifferent analyses are stored in the Method menu. These methods haveavailable all resources defined in the Setup menu.RunThe titration is performed in the Analysis menu. The method you call updetermines the analysis sequence: Before the start of the titration, thetitrator checks whether, e.g. the titrant defined in the method is also stored inthe Setup menu.SampleThe Sample menu is used for the entry of sample data, primarily for sampleseries, which can be performed automatically with a sample changer(sample data memory).Note: Each menu is further subdivided, i.e. it has several sets of operations which, depending on the task, are further subdivided. In this Quick Guide and in the ReferenceHandbook, these submenus are described as menus, lists or masks.8METTLER TOLEDO DL50/DL53/DL55/DL58

The titrator3.1.2The Auxiliary function keysTo measure the potential of a solution or rinse a burette, the required commands are alsoassigned to sets of operations (menus). As they are independent of a sample analysis, butcan act in a supporting role, we refer to these as auxiliary functions. They are accessibleunder the corresponding keys.You can measure the potential or the temperature of a solution and calibratethe temperature sensors.SensorYou can switch the stirrer on or off and change the stirring speed.StirrerYou can operate the sample changer manually.ChangerYou can rinse the burette, dispense a particular volume and titrate manually.Burette*ResultsYou can view the result list of analyzed samples and modify the statisticalevaluation of a series.You can print out additional reports.ReportMisc.DataTransfer3.1.3You can, among other things, define the date and language and activatecontrol inputs and outputs.You can copy data from the titrator to the memory card or transfer data to acomputer.The Command keysThe commands initiated with F1 . F5 change in accordance with the selected function.The following commands require an explanation:Esc: If you have made changes to the current menu or a submenu, they are discarded, inother words the original values/names are retained.OK:The command is always used as a confirmation for what you have done, e.g. changed a value have viewed, e.g. checked a list for completeness wish to do, e.g. rinse a burette wish to adopt, e.g. a name or value from a selection menu.METTLER TOLEDO DL50/DL53/DL55/DL589

The titratorModify: When this command appears, F4 can be used to show a submenu that can or must be modified show a selection menu from which you can or must adopt values or names change an existing parameter value or name directly.Note: If a value (name) can be modified or entered only with the keyboard, thiscommand does not appear.3.1.4ShiftCEDelShiftShiftThe Entry keysWith the Shift key you can activate the characters associated with the numeric keys.Del: You delete the number/symbol/letter at the cursor position.CE: You clear the entry in a line. 74You move the cursorto the rightor to the left.MethodsMETHODMethod IDStandard methodsUser methodsDelete90001 PrintModifyCursor (flashes)Key combinationsWith the Shift and Command keys (key combinations) you can execute the followingcommands:Shift key jumps 4 display lines at a time upward. key jumps 4 display lines at a time downward.Shift F1 initiates a line feed on the printer. F2 initiates a form feed on the printer.Shift F3 : the current display is printed out (copied).Shift F4 : the system data are printed out (see Reference Handbook, Section 9).10(See Reference Handbook, Section 2.7.1.1)METTLER TOLEDO DL50/DL53/DL55/DL58

The titrator3.2Changing the languageShould you understand one of the available languages better than the one displayed, selectthis as follows:Misc.MiscellaneousMISC.Define titrator settingsAdjust measuring inputsShorten analysis sequence Titrator settingsDate/time formatDate/timeLanguageEscEsc– Press F5 .MISC.– Press the key twice to select "Language". ModifyLanguageActive languageOKOK– Then press F4 .MISC.– Press F4 repeatedly until, for example, "Español" appears.EnglishModifyConfiguración tituladorFecha/horaLenguaEncabenzamiento de informeID tituladorEscCambiarMETTLER TOLEDO DL50/DL53/DL55/DL58OKMISC. OKWith the two commands, Esc or OK, the mask"Titrator settings" reappears.Esc: The change you have made is discarded, i.e.the texts remain in English.OK: The change you have made is confirmed, i.e.the texts appear in Spanish.11

The first titration4.How to perform your first titrationWe will use a simple acid-base titration to explain the sequence of a titration method. Themethod for this acid determination is stored as the METTLER method entitled "Acid content"with the identification 90001:5 mL of an HCl solution (concentration 0.1 mol/L)are titrated with NaOH (concentration 0.1 mol/L).4.1Preparations– Prepare hydrochloric acid and sodium hydroxide with the above concentrations. Thesodium hydroxide must be free from carbonate.– Prepare the 10 mL burette for the sodium hydroxide and position on the second drive (seeillustration in Section 3).– To protect the sodium hydroxide against CO2, place a drying tube on the burette holder ofthe NaOH bottle filled with, e.g. "sodium hydroxide on support".– Fasten a titration beaker to the titration stand and insert the dispensing tube of the NaOHin one of the openings of the titration head.– Fill the burette (see overleaf).Wait until you have filled the burette before– attaching a pH electrode with a Lemo cable tothe sensor input and the stirrer to the output.(In the Setup menu, inputs and outputs are defined with the names "Sensor 1" and "Stirrer 1")Rear view of the titrator with pH option(detail)The attachment of a printer and/or a balance isdescribed in Section 2.7 of the Reference Handbook. For the actual analysis, there is no need toattach either.Stirrer output"Stirrer 1"12Input for referenceelectrodeSensor input"Sensor 1"METTLER TOLEDO DL50/DL53/DL55/DL58

The first titration4.1.1Filling (rinsing) buretteBuretteBuretteBURETTERinse buretteRinse tipDispense OKRinse buretteBurette driveEscBURETTEDrive 21)Modify1)Rinse buretteBurette drive– Press F5 .StartBURETTEDrive 2appears only with DL55 and DL58, as two burette drives can be installed.– Press F5 .The piston of the burette is moved upward and theair expelled. An initial small amount of sodiumhydroxide is siphoned in when the piston returns toits initial position. The display again shows:StopRinse buretteBurette driveEscBURETTEModify1)Rinse buretteBurette drive– Repeat the rinsing operation twice more to ensure the burette is completely filled and thetubes are well rinsed.Drive 2StartBURETTEDrive 2– Then remove the titration beaker and rinse thepropeller stirrer and dispensing tube with deionized water.– Press the Reset key: The initial mask appears.StopYou can stop the rinsing operation at any time with F5 .METTLER TOLEDO DL50/DL53/DL55/DL5813

The first titration4.2Performing titration method 90001– Add approx. 50 mL deionized water to a titration beaker, pipette in 5 mL of the preparedhydrochloric acid and fasten the beaker to the titration head.RunSamples to be analyzedNumber of samplesMethod IDUserRUN1– Enter 3 for the number of samples.StartSamples to be analyzedNumber of samples3Method IDUser– Enter 90001 for the method identification andthen press F5 or the Run key.Samples to be analyzedMethod ID90001UserModifyStirrer 1: Stand 1Sensor 1: DG111Drive 2: 0.1 mol/L NaOHPrintEsc– Press the key.RUNModifyDefined areThe following sequence is described for a series ofthree samples to allow the calculation of statisticaldata.Start(The identification of the method used to performthe last analysis is displayed.)RUNStartRUNOK– Enter your name (if a keyboard is attached) andpress F5 or the Run key.(The name used to perform the last analysis isstored as a suggestion.)Using this information, you should check whether the stirrer of titration "Stand 1" is attached to output "Stirrer 1", a pH electrode is attached to the input "Sensor 1"(DG111 is the METTLER TOLEDO pH electrode), the burette with the NaOH is located at "Drive 2".– Press F5 or the Run key.Sample No. 1Sample IDVolume [mL]0.0Limits [mL]4.0 - 6.0Correction factor f1.0RUN OKSample ID: You can enter an identification for thissample.The volume is the amount of sample that shouldbe titrated.The limit values are defined in the method andindicate that there are lower and upper limits to theamount of sample which should not be violated.Correction factor f: see Section 4.1 of the Reference Handbook.You can enter the temperature (line not shown) ofthe solution to be titrated.– Enter 5.0 as the volume of the first sample.– Press F5 or the Run key.14METTLER TOLEDO DL50/DL53/DL55/DL58

The first titrationCurrent sampleRUNNo. 1 of 3Sample IDMethod IDThis is the prompt or the last opportunity to fastenthe beaker with the first of the three definedsamples to the titration head.90001– Press F5 or the Run key.OKStir functionRUNWait time [s]Speed [%]The titrator stirs for 10 seconds at a speed of 50%to mix the solution (the elapsed time is displayed).10501)Hold1)Measured valuesRUN0.000 mL274.3 mVTableCurveReport functionHold1)RUNThe results of the first sample are then displayed. RUN – Remove the titration beaker with the first sample.– Rinse electrode, stirrer and dispensing tube withdeionized water.– Prepare the second sample and fasten the beaker to the titration head.– Enter 5.0 for the volume of the second sample.– Press F5 or the Run key.RUNNo. 2 of 3Sample IDMethod IDYou can view the third result with the key.The formulas for the calculations of these 3 resultsR1, R2 and R3 are defined in the method.– Press F5 or the Run key.OKCurrent samplePressing F2 displays the table of measured values, pressing F4 the titration curve "Potential vsVolume".If you have defined and attached a printer, thetitration curve and the table of measured values ofthis determination are printed out (see followingpages). The mask appears during this time.OKSample No. 2Sample IDVolume [mL]0.0Limits [mL]4.0 - 6.0Correction factor f1.0The titrator dispenses 2 mL in 3 steps and then titrates up to the specified maximum volume of7 mL.RUNOutput unit writing report.Result listMethod: 90001Sample 1R1 4.993 mL ConsumptionR2 0.1009 mol/L Acid contentappears only with DL55/DL58, i.e. you can press F5 to interrupt the titration.90001OKMETTLER TOLEDO DL50/DL53/DL55/DL58This is the prompt or the last opportunity to fastenthe second sample beaker to the titration head.– Press F5 or the Run key: The sequence forthe determination of the second and third samples is the same as for the first.15

The first titrationWhen the third sample has been analyzed and you have defined and attached a printer, thefollowing are printed out: the results of all three samples the table of measured values for the third sample and the Potential-Volume curve for the third sample.As soon as all data have been sent to the printer, the results of all samples and the statisticalcalculation for the NaOH consumption and HCl content appear in the display:ResultR3SampleR1R2list 3.675 g/L Acid content3 4.979 mL Consumption 0.1006 mol/L Acid contentUse the arrow keys to view all results.RUN You can then press either F5 or the Run key: Theanalysis menu remains active. OKReport of all results of the titrated samplesMethodMeasuredUser90001 Acid content18-Oct-1996 11:48C. De Caro01-Jul-199512:00ALL RESULTSNo.IDSample size and results1HCl5.0R1 4.993R2 0.1009R3 3.6805.0R1 4.987R2 0.1008R3 3.6755.0R1 4.979R2 0.1006R3 LConsumptionAcid contentAcid contentConsumptionAcid contentAcid contentConsumptionAcid contentAcid contentSTATISTICSNumber resultsR1Mean valueStandard deviationRel. standard deviationnxssrel STICSNumber resultsR3Mean valueStandard deviationRel. standard deviationnxssrel 33.6750.005440.148g/Lg/L%Acid contentAcid contentMETTLER TOLEDO DL50/DL53/DL55/DL58

The first titrationReport of the table of measured values of the last titrated sampleMethodMeasuredUser90001 Acid content18-Oct-1996 11:48C. De 0.0560METTLER TOLEDO .21611.23401-Jul-199512:00ChangepH1st 54:014:074:134:184:234:284:324:3617

The first titrationReport of the titration curve18METTLER TOLEDO DL50/DL53/DL55/DL58

Method concept5.The method conceptMethodMethodsMETHODMethod IDStandard methodsUser methodsDelete PrintModifyMethodsMethod IDStandard methodsUser methodsMETTLER methodsPress the key:METHODPrintOKMETTLER and standard methods are stored in the titrator in the factory. You can adapt themethods of both groups to meet the requirements of your analyses. The modified methodsare always stored as User methods.Standard methodsMETTLER methodsThese methods have been entered by usand can not be recalled for an analysisdirectly. They do not have a method ID(entification) needed by the Analysis menu. The method parameters are stored withdefault values which you first have tomodify in accordance with your application.– Confirm "Standard methods" with OK:These methods have been developed byus for particular applications to allow theappropriate analyses to be run immediately: You can recall each METTLER methodusing the method ID(entification) in theAnalysis menu, e.g. method 90001 (seeSection 4.2).– Use the key to select "METTLER methods" and press F5 :Method IDTitle of the methodTitle of the methodStandard methodsEquivalence point titr'nEnd point titration (EP)Titer by EQP titrationEscPrintMETHOD ModifyMETTLER TOLEDO DL50/DL53/DL55/DL58METTLER methods900019000290003EscAcid contentCalibration pH electrodeCalibration F- electrodePrintModifyMETHOD 19

Method conceptEach method comprises several substeps which we refer to as Functions. These functionsare executed in succession in the analysis (see Sections 6.2 and 7.3).Each function comprises Parameters, which define the actual task of the function. You canmodify these parameters.5.1METTLER methodsThe DL50 has 4, the DL53 20 and the DL55 and DL58 30 METTLER methods stored. Allthese methods are described in the enclosed brochure "30 Selected Applications forMETTLER TOLEDO Titrators DL50/DL53/DL55/DL58".METTLER methods900019000290003Esc5.2Acid contentCalibration pH electrodeCalibration F- electrodePrintModifyPrint: Method 90001 is printed out with its functionsand parameters.METHODModify: The functions of method 90001 appear.Press F1 , Esc: The method groups reappear. Standard methodsIn all four titrators, 21 standard methods are stored under a title. Number and sequence ofthe functions are given for each method.123Equivalence point titr'nTitleSampleStirEQP d point titration (EP)TitleSampleStirEP ter by EQP titrationTitleSampleStirEQP titrationCalculationTiterReport45Titer by EP titrationTitleSampleStirEP titrationCalculationTiterReport20Sensor ationReport6Sensor ationReportMETTLER TOLEDO DL50/DL53/DL55/DL58

Method concept7Learn titrationTitleSampleStirLearn tat lationCalculationReport10Blank by EP titrationTitleSampleStirEP titrationCalculationCalculationAuxiliary valueReport112 Step titration (EQP)TitleSampleDispenseStirEQP QP titrationCalculationCalculationReport13EQP titr'n with dispenseTitleSampleDispenseStirEQP EP titration with dispenseTitleSampleDispenseStirEP TTLER TOLEDO DL50/DL53/DL55/DL589Blank by EQP titrationTitleSampleStirEQP titrationCalculationCalculationAuxiliary valueReport122 Step titration (EP)TitleSampleDispenseStirEP P titrationCalculationCalculationReport15Combined EP/EQP titr'nTitleSampleStirEP titrationCalculationCalculationReportEQP titrationCalculationCalculationReport21

Method concept161817EQP titration (Ipol/Upol)TitleSampleStirEQP titration Titer (EQP Ipol/Upol)TitleSampleStirEQP titration (Ipol/Upol)CalculationTiterReportBlank (EQP Ipol/Upol)TitleSampleStirEQP titration (Ipol/Upol)CalculationCalculationAuxiliary valueReport192021EP titration (Ipol/Upol)TitleSampleStirEP titration Titer (EP Ipol/Upol)TitleSampleStirEP titration (Ipol/Upol)CalculationTiterReportBlank (EP Ipol/Upol)TitleSampleStirEP titration (Ipol/Upol)CalculationCalculationAuxiliary valueReportNote:You can perform the standard methods 16 through 21 only if you have installed aKF option (see Section 10.5 of the Reference Handbook).Application examples of the standard methods221 Equivalence point titration (EQP)For titrations to the equivalence point, e.g. acid/base, redox,argentometric and complexometric titrations2End point titration (EP)For titrations to the end point, e.g. acid/basetitrations3Titer by EQP titrationTiter determination with an equivalence point titration, e.g.acid/base, redox, argentometric and complexometric titrations4Titer by EP titrationTiter determination with an end point titration5Sensor calibrationCalibration of pH and ion selective electrodes6Sensor measurementConcentration measurement with ion selective electrodes7Learn titration(see Section 3.3.8 of the Reference Handbook)METTLER TOLEDO DL50/DL53/DL55/DL58

Method concept8Stat titrationpH- or mV-stating, e.g. solution and enzyme kinetics9Blank by EQP titrationBlank value

METTLER TOLEDO DL50/DL53/DL55/DL58 3 Introduction 1. Introduction The METTLER TOLEDO DL50, DL53, DL55 and DL58 Titrators are microprocessor con-trolled analytical instruments which supply accurate and reproducible results thanks to their built-in intelligence. You can use the titrators to perform end point, equivalence point and pH-stat .File Size: 474KB

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