Operating Instructions. Titrator DL15

Transcription

1 Operating Instructions Titrator DL15

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3 Table of contents Table of Contents 1. Introduction 5 2. Safety measures 6 3. Standard equipment and Installation Standard equipment DL15 Titrator Installation Attaching the titration stand to the titrator Installing the burette Installing the magnetic stirrer Swiveling the titration stand Attaching and removing the titration beaker The titrator Design of the titrator Connections at the rear of the titrator The operating concept The display The arrow keys The function keys The input keys The menu keys The Help function keys The Escape key The Reset key The Home screen Setup Opening the Setup menu Titrants Adding a titrant Modifying a titrant Deleting a titrant Printing a titrant Titer determination from the titrant setup Sensors Adding a sensor Modifying a sensor Deleting a sensor Printing a sensor Sensor calibration from the sensor setup menu Sensor test from the sensor setup menu Peripherals Setting up a printer Setting up a balance Standards Adding a standard Modifying a standard Deleting a standard Printing a standard 39 METTLER TOLEDO DL15 I

4 Table of contents 5.6 Blank values Adding a blank value Modifying a blank value Deleting a blank value Printing blank values Blank value determination from the blank values setup menu Main methods Assignment of a function key Changing the assignment of a function key Deleting the assignment of a function key User management Adding a user Deleting a user Defining an active user Defining access rights Settings Setting the language Setting the date Setting the time Defining the temperature unit Entering the titrator ID Entering a report header Setting the beeper sound Titration stand Methods (Method) Starting a method Starting methods from the method editor Creating a method Modifying a method Sample Stir Measure EP titration Control param Recognition Termination param Evaluation Calculation Table of formulas for the calculation of results Report Deleting methods Printing a methods list Printing a method Predefined methods Series Starting a sample determination using the Series key Starting a titer determination using the Series key Starting a blank value determination using the Series key Analysis (Run) Starting a sample determination using the Run key Starting a titer determination using the Run key Starting a blank value determination using the Run key 80 II METTLER TOLEDO DL15

5 Table of contents 9. Performing a titration Preparations Filling the burette (rinsing) Performing titration method Auxiliary functions (Info, Sensor, Stirrer, Burette, Report, Results) Information menu Sensor Measuring temperature Measuring potential Calibrating a sensor Testing a sensor Stirrer Burette Rinsing the burette Rinsing the tip Dispensing Manual titration Report Results Displaying and printing results Statistics Terminating the series Error messages, malfunctions and hardware tests Global errors and malfunctions Hardware tests User interface Communication interfaces Auxiliary I/O ph input value Optional accessories and maintenance Optional accessories Service and maintenance Cleaning Disposal Technical data 109 Appendix: Predefined calibration standards 120 Index 124 METTLER TOLEDO DL15 III

6 Table of contents IV METTLER TOLEDO DL15

7 Introduction 1. Introduction The DL15 Titrator is the ideal solution for all requirements in the food industry, water/ wastewater analysis, and the chemical industry when all that is needed is an endpoint titration or a ph measurement. The DL15 is mainly used to determine the acid and base content of a sample. It features easy-to-understand intuitive user guidance so that, for example, pressing the Run button twice starts the method you last ran. The user can assign three other methods to individual function keys, making methods easy to find and start. The keys used for the most frequently used manual functions are identified by pictograms. Titrants and sensors can be selected from the instrument s database. Alphanumeric input is easily entered by means of a special keypad, just like with a mobile phone. There is no need to connect an external keyboard. The DL15 calculates the analytical results in predefined units and sends an analysis report to commercially available printers. METTLER TOLEDO DL15 5

8 Safety measures 2. Safety measures The titrators have been tested for the experiments and purposes documented in this Operating Instructions. This does not, however, absolve you from the responsibility of performing your own tests on the products supplied by us regarding their suitability for the methods and purposes you intend to use them for. Please adhere strictly to the following safety measures. Risk of an electrical shock Measures for your protection Make sure that the power cable supplied is plugged into a power outlet that is ground! A technical defect could otherwise have lethal consequences. Switch off the instrument and pull out the power cable before you open the instrument housing! An electrical shock could have lethal consequences. Risk of explosion Do not work in an environment subject to the risk of explosions! The instrument housing is not gastight (risk of explosion through spark formation, corrosion through the ingress of gases). Corrosive chemicals Make sure that the titration beaker is always securely attached in the titration head! If the beaker falls out, you could injure yourself when working with poisonous titrants and solvents, strong bases or acids. Caution When using chemicals and solvents, follow the manufacturers' instructions and the general rules for safety in the laboratory! Caution Measures for operational safety Have the instrument serviced only by METTLER TOLEDO Service! Wipe off any droplets of liquid! The instrument is not watertight. Eliminate the following environmental effects: strong vibrations, direct sunlight, humidity over 80%, temperatures below 5 C and over 40 C, strong electric or magnetic fields! 6 METTLER TOLEDO DL15

9 Standard equipment and Installation 3. Standard equipment and Installation 3.1 Standard equipment DL15 Titrator The parts are given with order number and the number of items supplied. For additional orders, some parts are only available as a minimum order quantity. In this case, the minimum order quantity is noted after the order number. The standard equipment and the optional accessories for the DV1020 burette are listed in the operating instructions for the interchangeable burette. This is supplied with the burette. Titrator Cap (2x) External power supply Dummy cover Power cable (country specific) (example) Titration stand, manual Holder for titration stand Spacing ring Fixing screw (for holder) Clamping ring Magnetic stirrer Threaded ring Magnetic stirrer bars DG115-SC Combined glass electrode with sleeve frit for titrations in aqueous media METTLER TOLEDO DL15 7

10 Standard equipment and Installation Triaxial cable SC-LEMO-60 (length: 60 cm) Stopper ST 7.5 (4x) (minimum order quantity 5 pcs.) Electrode sleeve (minimum order quantity 5 pcs.) Connection cable for HP compatible printer Titration vessel 100 ml polypropylene (2x) (set of 1400 pcs.) 2 g glass wool Drying tube holder Drying tube Interchangeable burette, complete (for further accessories: see operating instructions for the interchangeable burette) DV1020 DL15 Applications Brochure English Protective cover for keypad (minimum order quantity 3 pcs.) Operating Instructions English Stopper ST 14.5 (5x) (minimum order quantity 5 pcs.) 8 METTLER TOLEDO DL15

11 Standard equipment and Installation 3.2 Installation Attaching the titration stand to the titrator When the titration stand is delivered, the spacing ring, clamping ring and threaded ring are already mounted. The holder for the titration stand still has to be fixed to the titrator with the corresponding screw. Afterward, the assembled titration stand can be inserted from above. The diagram below shows how the titration stand is attached to the titrator and how the titration stand can be assembled and disassembled. Cap Titration stand Spacing ring Clamping ring Screw Threaded ring Titration beaker Holder for titration stand METTLER TOLEDO DL15 9

12 Standard equipment and Installation Installing the burette 1. Screw the burette with holder onto the titrant bottle (see operating instructions for burette. 2. Slide the burette onto the titrator: The slot on the cam and piston rod must be parallel plug-in unit. (If this is not the case, press the Reset key.) 3. Turn the arrestment knob in the direction shown by the arrow to fasten the burette. 4. Place the dispensing tube into one of the openings in the titration stand. When you rinse the burette and tubing, place the dispenser tube in a waste container! Fixing screw for titration stand holder Cam Arrestment knob Piston rod of the burette drive Installing the magnetic stirrer The titrator has a slot on the right side of the housing into which the METTLER TOLEDO magnetic stirrer can be inserted as shown in the following diagram. The magnetic stirrer is inserted into the slot of the titrator from the right so that it slides into the guide rail. The connection cable of the magnetic stirrer is guided out to the rear in the slot on the right side of the housing between the housing and the holder for the titration stand. To do this you may have to briefly remove the holder for the titration stand. The connection cable of the magnetic stirrer is connected to the "Magnetic stirrer" connection at the rear side of the housing. The arrow on the mini-din plug must point toward the head of the screw. Magnetic stirrer 10 METTLER TOLEDO DL15

13 Standard equipment and Installation Swiveling the titration stand The titration stand can be swiveled in order to work with the magnetic stirrer. If the compact stirrer is used, it is advisable to use the titration stand in the swiveled position. You can swivel the titration stand in and out. To do this, you lift the titration stand slightly and pull it upward a little bit out of the holder. Now you can swivel it to the desired position and then let it slide back into the holder. METTLER TOLEDO DL15 11

14 Standard equipment and Installation Attaching and removing the titration beaker To insert a titration beaker in the titration stand, you must first make sure that the threaded ring is loose (a quarter to half a turn is sufficient). Then, carefully insert the titration beaker from below into the titration stand A, and tighten the threaded ring B. To remove the titration beaker from the titration stand, loosen the threaded ring about a quarter to half a turn C, and then carefully remove the titration beaker downward out of the titration stand. 12 METTLER TOLEDO DL15

15 The titrator 4. The titrator 4.1 Design of the titrator Burette Arrestment knob Titrant bottle Titrator stand Sample beaker Magnetic stirrer Keypad 4.2 Connections at the rear of the titrator mv / ph electrode Overhead stirrer Reference electrode Temperature sensor Polariz. electrode Magnetic stirrer RS-P42 printer Balance not assigned Rondolino HP compat. printer Power supply METTLER TOLEDO DL15 13

16 The titrator The following devices can be connected to the corresponding interfaces: Connection mv/ph Ref PT1000 Pol Overhead Stirrer Magnetic Stirrer Balance Rondolino TTL I/O RS-P42 Computer Printer 5V/24V DC Device mv / ph electrode (sensor) Reference electrode PT1000 temperature sensor polarized electrode (sensor) Overhead stirrer Magnetic stirrer Balance (RS232C) Rondolino, external devices RS-P42 (GA-42) printer (RS232C) not assigned HP-compatible printer (Centronics) Power supply 4.3 The operating concept The operating console of the titrator consists of the display in the middle with several groups of keys arranged around it. The various functional areas are described in the following sections. 14 METTLER TOLEDO DL15

17 The titrator The display The display consists of four different elements. The title line across the top shows the name of the menu (B) and submenu (A) that you are currently using, or the name of the screen. On the right-hand side of the screen there is a scroll bar (D). This has a small black bar that represents the portion of the menu shown on the display. You can move the visible part of the menu upward or downward through the display area using the arrow keys. The black-inverted line (C) always displays the current selection. The three black-inverted boxes (E) across the bottom line of the display show the functions to which the function keys directly below (F1, F2 and F3) are assigned for the menu item selected The arrow keys The arrow keys are located on the right of the display. You can use these to move the black scroll bar up or down within a menu to select a menu item. If you simultaneously press an arrow key and the Shift key (arrow pointing upward), the scroll bar is shifted upward (or downward) three lines The function keys The function keys are located directly below the display. Their assignment depends on the particular menu item selected and is shown by the three black-inverted boxes across the bottom line of the display, for example, Print for the command to print, or OK to confirm a selection or a change The input keys The input keys are located on the right-hand side of the operating console. They allow alphabetical, numerical and special characters to be entered. Entering character strings into text boxes To enter a number or one of the letters written above a number, press the corresponding number key repeatedly until the desired character appears in the display. After a short pause, the cursor jumps one step further for you to enter the next character. METTLER TOLEDO DL15 15

18 The titrator - Pressing the number key 2 once, for example, writes the letter "a"; pressing it three time, the letter "c", and so on. - To obtain large characters, you must press and hold down the Shift key (arrow pointing upward) while selecting the character. - You can delete the last character by pressing the Del key. If you simultaneously press the Delete key and the Shift key, the entire content of the text box is deleted. - To insert a space, press the number key 0. - You can insert special characters by simultaneously pressing the number key 1 and the Shift key. A screen appears displaying all the available special characters. The black box indicates the character currently selected. - Select the desired character using the arrow keys and the < and > keys. - Press OK to enter the special character in the text area. Entering numbers into number boxes Only numbers, a point, and a minus sign can be entered into number boxes. - To enter a number, press the desired number key. - To enter a negative sign, simultaneously press the. and the Shift keys The menu keys Using the menu keys, you can call up the four main menus of the titrator. Each of these three menus has a particular assignment for performing an automatic analysis. The Setup key opens the Setup menu of the titrator. All the resources such as titrants, sensors, standards and blank values necessary for the titration are stored and managed in this menu. In addition, you can select the internal titrator settings you require and configure peripheral devices. The Method key opens the Method menu of the titrator. The methods stored in the titrator are managed in this menu. You can store your own methods, delete and modify them. A number of methods developed by METTLER TOLEDO are already stored and can be directly used to perform analyses or be used as templates for new methods. The resources you want to use for a method must be defined and stored beforehand in the Setup menu. The Run key opens the Start menu to perform an analysis. Methods used for different determinations can be selected and started. The Series key opens the start menu to perform a sample series analysis. Methods used for different determinations can be selected and started An automation of the series determination can be achived by using a Rondolino sample changer. 16 METTLER TOLEDO DL15

19 The titrator The Help function keys The Help function keys let you access functions that are not directly involved in performing a sample analysis, but nevertheless in some way support it (hence the name Help functions). Examples of such functions are the rinsing of burettes, the calibration or testing of a sensor or the display and management of analytical results. This menu lets you measure the ph, potential or temperature of a solution and test and calibrate ph and ISE sensors. The burette and the burette tip can be rinsed, and any volume you like dispensed. You can perform a manual titration. The variable speed stirrer can be switched on and off. You can view the titrator information and open a menu to test the titrator hardware and the connected devices. You can view, print and manage the results of your analyses including statistical evaluations. In the Report menu you can define and print additional reports The Escape key By pressing the Escape key, you can quit a menu or a selection at any time and discard the changes you made. You always return to the previous menu and the original values and names remain the same The Reset key Pressing the Reset key terminates analyses, rinsing or dispensing processes, and other actions. The titrator is then reset and you return to the Home screen. Data that was not saved beforehand is lost. METTLER TOLEDO DL15 17

20 The titrator The Home screen The Home screen appears on the display as soon as you switch on the titrator. It is the starting point for operating the titrator. Each time you reset the titrator by pressing Reset, you return to the Home screen. The screen displays the following important information: the current date and time. the current user. (See "5.8.3 Defining an active user") the access rights for the active user: Expert or Routine. (See "5.8.4 Defining access rights for active users") the assignment of the F1, F2 and F3 function keys with the main methods. (See "5.7 Main methods") 18 METTLER TOLEDO DL15

21 Setup 5. Setup In this chapter you learn how to set up the titrator for your specific requirements. To perform a titration, you must first define and configure the resources (titrants, sensor, peripherals, etc.) used for the method in the titrator. 5.1 Opening the Setup menu - Press the Setup button to open the Setup menu. - A list of the resources appears. You can scroll the list upward or downward using the arrow keys on the right next to the display. The black-inverted line always shows the current selection. If you press Print, the list with the available entries for the selected resource is printed. See "5.4.1 Setting up a printer" If you press OK, the list of the selected resources appears on the display. 5.2 Titrants - Press Setup to open the Setup menu. - Select "Titrant" using the arrow keys and press OK to confirm. The list of the titrants stored in the titrator appears. The titrants used by the METTLER methods are already preset in the titrator. You can delete titrants, and modify or print the parameters of the selected titrants. Furthermore, you can determine and store the titer for each titrant using an automatic function. You can add a new titrant by modifying the parameters of an existing titrant and then storing it under a new name. A maximum of 30 titrants can be stored in the titrator. METTLER TOLEDO DL15 19

22 Setup Adding a titrant Proceed as follows to define a new titrant: - Press Setup to open the Setup menu. - Select "Titrant" using the arrow keys and press OK to confirm. The list of the titrants stored in the titrator appears. - Select an existing titrant from the list of titrants and press Modify. - Change the name to the name of the new titrant you want to define. - Change the parameters of the titrant corresponding to the new titrant you want to define. See "5.2.2 Modifying a titrant". - Press Save to confirm the changes you have made. - The new titrant appears in the list. You can discard the changes you have made by pressing Esc to quit the selection. In this case, the titrant is not stored. Determine the titer of the new titrant using the automatic titer determination (Titer key) if you have not already entered it manually. See "5.2.5 Titer determination from the Titrant setup". In any case, first change the name of the titrant. Otherwise the changes you made for the existing titrant will be effective on pressing the Save key, and no new titrant will be stored in the titrator! Modifying a titrant - Press Setup to open the Setup menu. - Select "Titrant" using the arrow keys and press OK to confirm. The list of the titrants stored in the titrator appears. - Select the titrant whose parameters you want to change. - Press Modify. - The list of parameters of the selected titrant appears and the individual parameters can be selected and changed. - Press Save to accept your changes and quit the menu, or press Esc to discard your changes and quit the menu. All titrants contain the following parameters: 20 METTLER TOLEDO DL15

23 Setup Name Conc. [mol/l] Titer Minimum Maximum Titer Standard Burette The name of the titrant. The concentration of the titrant in [mol/l]. The titer can be automatically determined using a titer determination, or manually entered. If the titer is determined through a titer determination, the current date and time are stored. The "Minimum" parameter lets you define the lower limit for the range within which the titer must be. The "Maximum" parameter lets you define the upper limit for the range within which the titer must be. This parameter indicates whether the titer determination was automatically determined ("Determined") or manually entered ("Edited"). Here you can select one of the standards defined in the titrator to determine the titer of your titrant. Using this parameter you can define the burette volume. Possible values are 1, 5, 10 and 20 ml. Charge Fill rate [%] Check after [day] Expiry Date Time With this parameter you can record information about the batch from which the titrant originates. The "Fill rate" indicates how quickly the burette is filled with titrant. Filling the burette at the highest rate corresponds to a fill rate of 100%, and at the lowest rate to a fill rate of 30%. The preset value is 100% This value is used to calculate the expiration date for the titrant. A period of 0 to 100 days can be defined. If the parameter has the value 0, no expiration date is determined. If the value 0 is entered for the "Check after" parameter, no expiration date is calculated. The date of the last titer determination. Each time you store the titrant, the date is set to The time of the last titer determination. Each time you store the titrant, the time is set to 00:00. METTLER TOLEDO DL15 21

24 Setup If you change the name of a titrant and save your changes, a new titrant is created under the new name. If the value for the titer determined by a titer determination or the manually entered value is outside the range defined by "Minimum" and "Maximum", an error message appears and the titer must either be determined or entered again. When you use a titrant of higher viscosity, it is advisable to reduce the fill rate in order to prevent air being sucked-in when filling the burette. If, at the start of an analysis, the titant has expired (the expiration date has been exceeded), a message appears to draw your attention to this. If you still want to perform the determination, you must confirm the message. In the report, a corresponding line appears that notes that the titrant has expired Deleting a titrant - Press Setup to open the Setup menu. - Select "Titrant" using the arrow keys and press OK to confirm. The list of the titrants stored in the titrator appears. - Select the titrant you want to delete. - Press Delete. - In the dialog that follows, you are asked whether you really want to delete the selected titrant. Confirm deletion by selecting "Yes" and pressing OK, or terminate deletion by selecting "No" and pressing OK to confirm. You can only delete titrants that have not been used in a method. Titrants referenced by METTLER methods cannot be deleted. 22 METTLER TOLEDO DL15

25 Setup Printing a titrant - Press Setup to open the Setup menu. - Select "Titrant" using the arrow keys and press OK to confirm. The list of the titrants stored in the titrator appears. - Select the titrant whose parameters you want to print. - Press Print. - The parameters of the selected titrant are printed on the printer as soon as you confirm by pressing OK Titer determination from the titrant setup The accuracy of the results of your analysis depends on the accuracy with which you determine the concentration of your titrant. When you prepare a titrant, a number of errors can occur that cause the actual concentration (C actual ) to deviate from the desired concentration (C nom ) of your titrant. The quotient of the actual concentration of the titrant and its desired concentration is called the titer of the titrant: t = c actual c nom In the ideal case, C actual = C nom and the titer, t, is 1. If the concentration of the titrant is too high, t is > 1. If the concentration of the titrant is too low, t is <1. The titer enables the titrator to calculate the results of your analyses corresponding to the actual concentration of the titrant used. It is therefore essential for you to accurately determine the actual concentration of the titrant against a reference substance before you first use it. The titrator can store the corresponding titer as a parameter for every titrant defined in the titrator. As long as the titer for a titrant has not been determined, the default value 1 is used. You can determine the titer yourself, enter the value for the titrant manually in the Setup menu, or to determine it through automatic titer determination with the titrator. Before doing this, you should make sure that a suitable standard is already stored in the titrator for the primary standard you want to use. If this is not the case, you must first define a new standard in the instrument. See "5.5.1 Adding a standard". METTLER TOLEDO DL15 23

26 Setup Performing the titer determination from the Titrant setup - Press Setup to open the Setup menu. - Select "Titrant" using the arrow keys and press OK to confirm. The list of the titrants stored in the titrator appears. - Select the titrant whose titer you want to determine. - Press Modify. - Select "Standard". - Check whether the parameters of the selected standards match your primary standard substance. If this is not the case, press Modify and select the suitable standard from the list of standards stored in the titrator. Press OK to confirm your selection. - Press Titer to open the titer determination function. - A list of the methods appears. It shows only methods that use the titrant whose titer you want to determine. - Select a suitable method using the arrow keys and start the titer determination by pressing Start. - The titer determination is performed according to the conditions predefined for the method used. (See "6.3 Modifying a method"). The calculations from the method are ignored. The sample data from the method is replaced with default data. - After the determination, you can view the statistics of the current sample series by pressing Stat.. - If the titer determined in this way is within the defined limits, press Save to accept the result of the titer determination (or the mean results if you have performed the titer determination several times). - The date and time of the last titer determination are automatically updated. - Quit the display that follows by pressing Esc. in order to prevent the date and time being set to and 00:00. It is also possible to perform the automatic titer determination from the Analysis menu. See "8.2 Starting a titer determination using the Run key" The concentration of a titrant can change after you have determined the titer. It is therefore absolutely essential to determine the titer at regular intervals in order to guarantee constant accuracy of the analysis results. The titrator can also generate a specific expiration date for each titrant, which requests the user to determine the titer again after a certain period. 24 METTLER TOLEDO DL15

27 Setup 5.3 Sensors - Press Setup to open the Setup menu. - Select "Sensors" using the arrow keys and press OK to confirm. The list of sensors stored in the titrator appears. Some sensors are already predefined in the titrator. You can add new sensors, change them or delete them from the list. For ph and ISE sensors you can also perform an automatic sensor calibration. You can define: mv sensors ph sensors ion selective sensors (ISE) polarized sensors To add a new sensor, you must change the parameters of one of the existing sensors and then save it under a new name. A maximum of 20 sensors can be stored in the instrument Adding a sensor To define a new sensor, proceed as follows: - Press Setup to open the Setup menu. - Select "Sensors" using the arrow keys and press OK to confirm. The list of sensors stored in the titrator appears. - Select an existing sensor from the list of sensors and press Modify. - Change the name to the name of the new sensor you want to define. - Change the parameters of the sensors according to the new sensor you want to define. See "5.3.2 Modifying a sensor". - Press Save to confirm your changes. - The new sensor appears on the list. You can discard your changes at any time by pressing Esc to quit the selection. In this case the sensor is not stored. METTLER TOLEDO DL15 25

28 Setup Before using it for the first time, you must calibrate a newly defined ph or ISE sensor using the automatic calibration function (the Calib. key) if you have not already manually entered the slope and zero point. See "5.3.5 Sensor calibration from the sensor setup menu". In any case, first change the name of the sensor. Otherwise when you press Save, your changes will be effective for the existing sensor and no new sensor is stored in the instrument! Modifying a sensor - Press Setup to open the Setup menu. - Select "Sensors" using the arrow keys and press OK to confirm. The list of sensors stored in the titrator appears. - Select the sensor whose parameters you want to change from the list of sensors. - Press Modify. - The list of parameters of the selected sensor appears; the individual parameters can be selected and changed. - Press Save to accept your changes and to quit the menu, or press Esc to discard your changes and quit the menu. The following parameters can be changed, depending on the type of sensors: Name Input The name of the sensor. Depending on the type of sensor, either the ph or the pol. input can be selected to connect the sensor. (see "4.2 Connections at the rear of the titrator") Type This parameter lets you define the sensor type for sensors at the ph input. There is a choice of ph, mv and ISE. Unit A possible unit can be selected for the sensor (ph, mv or px). This appears only for ph and ISE sensors! SNR The serial number of the sensors can be entered here. Zero point [ph] or Zero point [px] The zero point of the ph or ISE sensor used. This value can be entered manually or be determined by the instrument during automatic sensor calibration. Prior to the initial calibration, the default value of 7.00 for ph sensors and ISE sensors is stored here. This appears only for ph and ISE sensors! Slope [mv/ph] or Slope [mv/px] The slope of the ph or ISE sensor used. This value can be entered manually or be determined by the instrument during the automatic sensor calibration. Prior to the initial calibration, the default value of for ph sensors is stored here. This appears only for ph and ISE sensors! 26 METTLER TOLEDO DL15

29 Setup Min. [mv/ph] or Min. [mv/px] Max. [mv/ph] or Max. [mv/px] Temperature [ C], [ F] or [K] Calib.. Check after [day] Expiry Min. defines the lower limit for the tolerance range within which the slope must be. For a ph sensor, the default value is The upper limit is correspondingly defined by Max. This appears only for ph and ISE sensors! Max. defines the upper limit for the tolerance range within which the slope must be. For a ph sensor, the default value is The lower limit is correspondingly defined by Min. This appears only for ph and ISE sensors! The measurement temperature can be specified here. This appears only for ph and ISE sensors! This parameter indicates whether the calibration was automatically determined ("Determined") or manually entered ("Edited"). This value is used to calculate the time for the next calibration of the sensor. A period of 0 to 100 days can be defined. If this parameter has the value 0, no date is set for the calibration of the sensor. This appears only for ph and ISE sensors! The "Check after" parameter sets the expiration date for the sensor, which indicates the time when the sensor has to be recalibrated. If only the value 0 is entered for the "Check after" parameter, then no expiration date is calculated. This appears only for ph and ISE sensors! Date The date of the last sensor calibration. This date is reset to each time the sensor is stored. This appears only for ph and ISE sensors! Time The time of the last sensor calibration. This time is reset to 00:00 each time the sensor is stored. This appears only for ph and ISE sensors! Test data Pressing the Test key opens the sensor test data. This appears only for ph and ISE sensors! METTLER TOLEDO DL15 27

30 Setup If you change the name of a sensor and save the changes, a new sensor with a new name is created. The parameters that appear in the list depend on the type of sensor. For ph, mv, ISE sensors and the phototrode, the ph input must be chosen; for polarized sensors, the pol. input. Prior to the first ph sensor calibration, the date and expiration date are and the time 00:00. The value for "Check after" is set to 0 days, and zero point and slope are set to the default values Deleting a sensor - Press Setup to open the Setup menu. - Select "Sensors" using the arrow keys and press OK to confirm: The list of sensors stored in the titrator appears. - Select the sensor you want to delete from the list. - Press Del. - In the dialog that follows you are asked whether you really want to delete the selected sensor. Confirm deletion by selecting "Yes" and pressing OK, or terminate the deletion process by selecting "No" and pressing OK to confirm. You can only delete a sensor that has not been used in a method Printing a sensor - Press Setup to open the Setup menu. - Select "Sensors" using the arrow keys and press OK to confirm. The list of sensors stored in the titrator appears. - Select the sensor you want to print. - Press Print. - The parameters of the selected sensor are printed on the printer as soon as you press OK to confirm. 28 METTLER TOLEDO DL15

31 Setup Sensor calibration from the sensor setup menu Zero point and slope E E 0 The calibration parameters of a ph electrode are the zero point ph 0 (ph at a potential of 0 mv) and the slope. The theoretical values of a ph electrode are stored in the titrator: +mv 0 ph ph Zero point = 7.0 [ph] and Slope = [mv/ph]. -mv The ph calculation is performed according to the following equation: mv signal ph=ph 0 + slope The slope is corrected for temperature in the calculation of the ph. E The sensor should be calibrated in order to obtain correct values for your electrode. The theoretical values are then automatically overwritten with the calculated calibration data during the calibration. If you only calibrate your electrode with one buffer solution, only the electrode zero point is recalculated. (Not possible with the titrator.) +mv 0 -mv ph MP ph E +mv MP With a two- or multiple-point calibration, the zero point and slope are calculated using linear regression. 0 ph 0 (MP) ph -mv MP METTLER TOLEDO DL15 29

32 Setup Performing sensor calibration from the sensor setup menu - Press Setup to open the Setup menu. - Select "Sensors" using the arrow keys and press OK to confirm. The list of sensors stored in the titrator appears. - Select the sensor you want to calibrate. - Press Modify. - Press the Calib.. - The setup menu for sensor calibration with the parameter list appears. Name The name of the sensor. Buff. type Number of buffers Speed [%] Temp. sensor The type of buffer solutions to be used for the calibration. You can select: ph (to define yourself) px (to define yourself) DIN/NIST DIN Fluka Merck MT-EU MT-USA Fisher JIS For the temperature dependencies of the buffers, see "Appendix A: Predefined calibration standards". With this parameter you can define the number and type of buffer solutions to be used for the calibration. The stirrer speed. Either the PT1000 temperature sensor can be selected or the temperature can be entered manually under the parameter "Temperature". Temperature de [mv] dt [s] The temperature during the sensor calibration. With this value the temperature-corrected slope of the ph electrode is used in the calculation of the ph. Appears only when the parameter "Temp. Sensor" is set to "Manual". During dt, the drift of the electrode potential must be less than de/dt [mv/s] in order to be accepted as measured value. This occurs in an interval defined by t(min) and t(max). t(min) [s] t(max) [s] Report The measured value is not accepted before t(min). The measured value is in any case accepted after t(max). You can select whether you want a report to be printed on the printer or not. 30 METTLER TOLEDO DL15

33 Setup - Select "Buff. type" using the arrow keys. Then press Modify and select the buffer type you are using. - Select "Number of buffers " and press Modify. - Add the desired number of buffer solutions to the buffer list using Add. You can select these from a list and then press OK to include them in the buffer list. (You can remove buffers again from the list by selecting them and pressing Delete.) - When you have defined the desired number of buffer solutions, press OK to return to the setup menu for the calibration. - Select "Speed [%]" and enter the speed for the stirrer in percent. - Select "Temp.sensor", press Modify and select the "PT1000" temperature sensor or "Manual". - If you have selected "Manual" for "Temp.Sensor", select "Temperature" and enter the temperature in the corresponding units. - Select "de [mv]" and enter the millivolt number for the determination of the maximum drift de/dt [mv/s] of the electrode potential. - Select "dt [s]" and enter the time in seconds for the determination of the maximum drift de/dt [mv/s] of the electrode potential. - Select "t(min) [s]" and "t(max) [s]" one after the other and define the time at which the measured value at the earliest (tmin) and at the latest (tmax) is to be accepted. - Select "Report" and select "none" or "printer" for the report printout using Modify. - Start the sensor calibration by pressing Start. - For the selected number of buffer solutions, a message appears each time requesting you to prepare the corresponding buffer solution. You must confirm this by pressing OK to start the measurement with the corresponding buffer solution. - After all buffer solutions have been measured, a summary of the calibration results appears on the display with the following information: Name of the sensor Calibration "OK" / "not OK" measured slope [mv/ph] measured zero point [ph] If the measured slope is outside the limits defined for the sensor Min. [mv/ph] and Max. [mv/ph], "Calibration not OK" appears and the calibration results are not accepted. - If the measured slope lies within the limits defined for the sensor, the slope and zero point for the sensor can be accepted by pressing Save. The date and time for the calibration are automatically updated. - If "Printer" was selected for the "Report" parameter, a report of the sensor calibration is printed on the printer. - Quit the display that follows by pressing Esc. in order to prevent the date and time from being set to and 00:00. The sensor calibration can also be opened using the Sensor Help function key. (See: " Calibrating a sensor") For storing into Setup, the slope is converted to 25 C. METTLER TOLEDO DL15 31

34 Setup Sensor test from the sensor setup menu Using the "Test sensor" function you can perform a test for a ph or ISE sensor. The data determined in the test can be printed on the printer. Performing the sensor test from the sensor setup menu - Press Setup to open the Setup menu. - Select "Sensors" using the arrow keys and press OK to confirm. The list of sensors stored in the titrator appears. - Select the sensor you want to test. - Press Modify. - Select "Test data" and press Test. - The setup menu for the sensor test appears with the parameter list. 32 METTLER TOLEDO DL15

35 Setup Name Buff. type Number of buffers Speed [%] Max. drift [mv/min] Temp. sensor Temperature de [mv] dt [s] t(min) [s] t(max) [s] Output The name of the sensor. The type of the buffer solutions to be used for the test. You can select: ph (to define yourself) px (to define yourself) DIN/NIST DIN Fluka Merck MT-EU MT-USA Fisher JIS This parameter lets you define the number of buffer solutions to be used for the sensor test. Two buffer solutions must be selected. The stirring speed of the stirrer. The maximum allowable drift in [mv/min]. Determines the maximum value for the drift determined by the test in [mv/ min]. You can select the PT1000 temperature sensor or enter the temperature manually under the parameter "Temperature". The temperature during the sensor tests. This value is used to correct the slope of the ph electrode for temperature and is taken into account in the calculation of ph. It appears only if the parameter "Temp. sensor" is set to "Manual". During dt, the drift of the electrode potential must be less than de/dt [mv/s] in order to be accepted as a measured value. This occurs in a period defined by t(min) and t(max). The measured value is not accepted before t(min). The measured value is in any case accepted after t(max). You can select "Printer" or "None". METTLER TOLEDO DL15 33

36 Setup - Using the arrow keys, select "Buff. type". Then press Modify and select the buffer type you are using. - Select "Number of buffers " and press Modify. - Add two buffer solutions to the buffer list using Add. You can select these from a list and then press OK to include them in the buffer list. (You can remove the buffers again from the list by selecting them and then pressing Delete.). - Press OK to return to the setup menu for the sensor test. - Select "Speed [%]" and enter the speed for the stirrer in percent. - Select "Max. Drift [mv/min]" and enter a value in [mv/min] that the drift must not exceed. - Select "Temp. sensor", press Modify and select the "PT1000" temperature sensor or "Manual". - If you have selected "Manual" for "Temp. Sensor", select "Temperature" and enter the temperature in the corresponding units. - Select "de [mv]" and enter the millivolt number for the determination of the maximum drift de/dt [mv/s] of the electrode potential. - Select "dt [s]" and enter the time in seconds for the determination of the maximum drift de/dt [mv/s] of the electrode potential. - Select "t(min) [s]" and "t(max) [s]" one after the other and define the time at which the measured value at the earliest (tmin) and at the latest (tmax) is to be accepted. - Start the sensor test by pressing Start. - For the two selected buffer solutions a message appears each time requesting you to prepare the corresponding buffer solution. You must confirm this by pressing OK to start the measurement with the corresponding buffer solution. - After the measurements have been performed for both buffer solutions, the drift is determined for a period of 60 seconds. If you have selected "Printer" under the menu item, the results of the sensor test are recorded on the printer. There follows the summary of the results of the sensor test on the display with the following information: Name of the sensor Drift "OK" / "not OK" Slope "OK" / "not OK" Drift [mv/min] Zero point [ph] Slope [mv/ph] 34 METTLER TOLEDO DL15

37 Setup If the measured slope or the measured drift is outside the limits defined for the sensor, then "Drift not OK" or "Slope not OK" appears. - The sensor test was successful if "OK" appears for both for the drift and the slope. The sensor test can also be opened using the Sensor Help function key. (See " Testing a sensor") 5.4 Peripherals - Press Setup to open the Setup menu. - Select "Peripherals" using the arrow keys and press OK to confirm. The setup menu for the peripherals that can be connected to the titrator appears. The following peripheral instruments can be connected: Printer (GA 42, RS-P42, HP compatible) Balance (uni- or bidirectional) Proceed as follows to setup these peripheral instruments Setting up a printer - Press Setup to open the Setup menu. - Select "Peripherals" using the arrow keys and press OK to confirm. The setup menu for the peripheral instruments that can be connected to the titrator appears. - Select "Printer" and press Modify. - Select one of the printers from the list. - Press OK to accept your changes and quit the menu, or press Esc to discard your changes and quit the menu. The following printers can be selected: GA 42 RS-P42 HP compatible printer METTLER TOLEDO DL15 35

38 Setup If you have connected an HP compatible printer, you can also define the paper format for this printer. - Select "HP compatible" and press Modify. - In the menu that follows you can select the appropriate paper from the list of entries by pressing Modify. The following paper formats for HP compatible printers can be selected: 8 1/2 * 11" 8 1/2 * 12" A4 If your titrator is not connected to a printer, select "Not defined" and confirm by pressing OK Setting up a balance If you have connected a balance to the titrator, you can configure it in this menu. You can then transfer the value for the sample weight directly from the balance each time the titrator requests it by pressing Balance. - Press Setup to open the Setup menu. - Select "Peripherals" using the arrow keys and press OK to confirm. The setup menu for the peripheral instruments that can be connected to the titrator appears. - Select "Balance"and press Modify. - Using Modify you can define the type of communication between the titrator and the balance. - Press OK to accept your changes and to quit the menu, or press Esc to discard your changes and quit the menu. The following configuration possibilities can be selected for a balance: "unidirectional" (for unidirectional communication between titrator and balance) "bidirectional" (for bidirectional communication between titrator and balance) "Not defined" If your titrator is not connected to a balance, select "Not defined" and confirm with OK. For the METTLER TOLEDO AE, AG, AT, AX and XS balances, use the setting "Bidirectional" and the following balance settings: Baud rate: 2400, Data bits: 7, Parity: even, Handshaking: no. 36 METTLER TOLEDO DL15

39 Setup 5.5 Standards - Press Setup to open the Setup menu. - Select "Standards" using the arrow keys and press OK to confirm. The setup menu for the standards stored in the titrator appears, or "Template" if no standards are stored in the titrator. In this menu you can define and store primary standard substances using different parameters. These standards are needed by the titrator for the automatic titer determination and can be changed and also deleted again. A maximum of 20 standards can be stored in the titrator Adding a standard Proceed as follows to define a new standard: - Press Setup to open the Setup menu. - Select "Standards" using the arrow keys and press OK to confirm. The setup menu for the standards stored in the titrator appears, or "Template" if no standards are stored in the titrator. - Select an existing standard from the list of standards (or the template if no standard is stored) and press Modify. - Change the name to the name of the new standard you want to define. - Change the parameters of the standard (or the template) according to the new standard you want to define. See "5.5.2 Modifying a standard". - Confirm your changes finally by pressing Save. - The newly defined standard appears in the list. - You can discard your changes at any time by quitting the selection by pressing Esc. In this case, the standard is not stored Modifying a standard - Press Setup to open the Setup menu. - Select "Standards" using the arrow keys and press OK to confirm. The setup menu for the standards stored in the titrator appears. - Select the standard whose parameters you want to change. - Press Modify. - The list of parameters of the selected standard appears; the individual parameters can be selected with the arrow keys and changed. - Press Save to accept you changes and quit the menu, or press Esc to discard your changes and quit the menu. METTLER TOLEDO DL15 37

40 Setup The following parameters can be changed depending on the type of standard: Name Entry type Minimum [g] / [ml] Maximum [g] / [ml] Mol. m. [g/mol] Conc. [mol/l] Equivalent number z Here you can enter the name under which the standard is to be stored. As entry type you can select mass or volume, depending whether you want to add the standard as a weighed quantity or a measured volume during the automatic titer determination. With "Minimum" and "Maximum" you can define a range for the quantity of the standard to be added. Minimum defines the lower limit of this range. Depending on the selected entry type, Minimum is given in [g] or in [ml]. Using "Minimum" and "Maximum" you can define a range for the quantity of the standard to be added. Maximum defines the upper limit of this range. Depending on the selected entry type, Minimum is given in [g] or in [ml]. Enter the molar mass of the standards. This only appears if entry type mass is selected. Enter the concentration of the standard. This only appears if entry type volume is selected. Enter the equivalent number z of the standard. If you change the name of a standard and save your changes, a new standard is created under the new name. 38 METTLER TOLEDO DL15

41 Setup Deleting a standard - Press Setup to open the Setup menu. - Select "Standards" using the arrow keys and press OK to confirm. The list of standards stored in the titrator appears. - Select the standard you want to remove from the list. - Press Delete. - In the dialog that follows you are asked whether you really want to delete the selected standard. Confirm deletion by selecting "Yes" and pressing OK, or terminate the deletion process by selecting "No" and pressing OK. You can only delete standards that are not referenced by a titrant Printing a standard - Press Setup to open the Setup menu. - Select "Standards" using the arrow keys and press OK to confirm. The setup menu for the standards stored in the titrator appears. - Select the standard whose parameters you want to print. - Press Print. - The parameters of the selected standard will be printed on the printer as soon as you confirm by pressing OK. METTLER TOLEDO DL15 39

42 Setup 5.6 Blank values - Press Setup to open the Setup menu. - Select "Blank values" using the arrow keys and press OK to confirm. The list of blank values stored in the titrator appears, or the entry "Template" if no blank values are stored in the titrator. In this menu you can determine and store all the blank values for the solvents you use. These blank values are used for the calculation of the results of your analyses and can be changed or deleted here. A maximum of 20 blank values can be stored in the titrator Adding a blank value Proceed as follow to add a new blank value: - Press Setup to open the Setup menu. - Select "Blank values" using the arrow keys and press OK to confirm. The list of blank values stored in the titrator appears, or the entry "Template" if no blank values are stored in the titrator. - From the list of blank values, select an existing blank value (or the template, if no blank value is stored) and press Modify. - Under "Solvent", enter the name of the solvent whose blank value you want to define. - Change the parameters of the blank value (or the template) according to the new blank value you want to define. See "5.6.2 Modifying a blank value". - Press Save to confirm your changes. - The new blank value appears on the list. - You can discard your changes at any time by pressing Esc to quit the selection. In this case no blank values are stored. You can enter the blank value of the solvent manually or by means of the automatic blank value determination. See "5.6.5 Blank value determination from the blank values setup menu" Modifying a blank value - Press Setup to open the Setup menu. - Select "Blank values" using the arrow keys and press OK to confirm. The list of blank values stored in the titrator appears. - Select the blank value whose parameters you want to change. 40 METTLER TOLEDO DL15

43 Setup - Press Modify. - The list of the parameters of the selected blank value appears. Individual parameters can be selected and then changed. - Press Save to accept your changes and to quit the menu, or press Esc to discard your changes and quit the menu. The following parameters can be changed: Solvent Here you can enter the name of the name of the solvent whose blank value is to be stored. Blank value [mmol] The blank value of the solvent. This value can either be entered manually or determined by the titrator during the automatic blank value determination. If the blank value is automatically determined, the date and the time are automatically updated. Minimum [mmol] "Minimum" and "Maximum" let you define a range in which the blank value of the solvent must be. "Minimum" defines the lower limit of this range. Maximum [mmol] "Minimum" and "Maximum" let you define a range in which the blank value of the solvent must be. "Maximum" defines the upper limit of this range. Blank This parameter indicates whether the blanc value was automatically determined ("Determined") or manually entered ("Edited"). Volume [ml] Enter the volume of the solvent to be used. Check after [day] This value is used to calculate the expiration date for the blank value. A period of 0 to 100 days can be defined. If the value of this parameter is 0, no expiration date is calculated. Expiry The expiration date for the blank value. If no other value than 0 is given for the parameter "Check after", then no expiration date is calculated. Date The date of the last blank value determination. Each time the blank value is stored the date is set to Time The time of the last blank value determination. Each time the blank value is stored the time is set to 00:00. METTLER TOLEDO DL15 41

44 Setup If you change the name of a blank value and store your changes, a new blank value is created under the new name Deleting a blank value - Press Setup to open the Setup menu. - Select "Blank values" using the arrow keys and press OK to confirm. The list of blank values stored in the titrator appears. - Select the blank value whose parameters you want to delete. - Press Del.. - In the dialog that follows, you are asked whether you really want to delete the selected blank value. Confirm deletion by selecting "Yes" and pressing OK, or terminate the deletion process by selecting "No" and pressing OK. You can only delete blank values that are not referenced by a method Printing blank values - Press Setup to open the Setup menu. - Select "Blank values" using the arrow keys and press OK to confirm. The list of blank values stored in the titrator appears, or the entry "Template" if no blank values are stored in the titrator. - Select the blank value whose parameters you want to print. - Press Print. - The parameters of the selected blank value are printed on the printer as soon as you press OK to confirm. 42 METTLER TOLEDO DL15

45 Setup Blank value determination from the blank values setup menu - Press Setup to open the Setup menu. - Select "Blank values" using the arrow keys and press OK to confirm. The list of blank values stored in the titrator appears, or the entry "Template" if no blank values are stored in the titrator. - Select the blank value whose value you want to determine. - Press Modify. - Press Blank. - In the display that follows, the methods are shown that reference the blank through the parameter "Solvent". - Select one of the methods shown and press Start. - The blank value determination is performed according to the preset conditions of the method you use. (See "6.3 Modifying a method") - If "Printer" was selected for the parameter "Report", a report of the blank value determination is printed on the printer. - By pressing Stat. you can view the statistics of the current sample series. - If the blank value determined is within the defined limits, the value (or the mean value of the results if you have performed the blank value determination several times) can be accepted by pressing Save. The date and time for the blank value determination are then automatically updated. - Quit the display that follows by pressing Esc. to prevent the date and time from being set to and 00:00. You can also perform the automatic blank value determination from the Analysis menu. See "8.3 Starting a blank value determination using the Run key" 5.7 Main methods - Press Setup to open the Setup menu. - Select "Main methods" using the arrow keys and press OK to confirm. The Main methods setup menu appears. METTLER TOLEDO DL15 43

46 Setup Using the "Main methods" setup function, a total of three methods (METTLER or User methods) can be assigned to the function keys F1, F2 and F3. These methods can then be started directly from the Home screen by pressing the function keys. Methods can be assigned to the function keys in the setup menu for the main methods; the assignment can be changed or deleted Assignment of a function key - Press Setup to open the Setup menu. - Select "Main methods" using the arrow keys and press OK to confirm. The Main methods setup menu appears. - Select the function keys to which you want to assign a method. - Press Modify. - In the menu that follows, select either "User methods" or "METTLER methods" and press OK to confirm your selection. - In the next menu, select the desired method and press OK to confirm your selection. - In the Main methods setup menu, the number of the assigned method appears next to the corresponding function key. - Quit the Main methods setup menu by pressing OK, or select another function key if you want to change its assignment Changing the assignment of a function key - Press Setup to open the Setup menu. - Select "Main methods" using the arrow keys and press OK to confirm. The Main methods setup menu appears. - Select the function key to which you want to assign another method. - Press Modify. - In the menu that follows, select either "User methods" or "METTLER methods" and press OK to confirm your selection. - In the next menu, select the desired method and confirm your selection with OK. - In the Main methods setup menu, the number of the newly assigned method appears next to the corresponding function key. - Quit the Main methods setup menu by pressing OK, or select another function key if you want to change its assignment. 44 METTLER TOLEDO DL15

47 Setup Deleting the assignment of a function key - Press Setup to open the Setup menu. - Select "Main methods" using the arrow keys and press OK to confirm. The Main methods setup menu appears. - Select the function key whose assignment you want delete. - Press Del. - "Not assigned" now appears next to the selected function key. - Quit the Main methods setup menu by pressing OK, or select another function key if you want to change its assignment. 5.8 User management - Press Setup to open the Setup menu. - Select "User management" using the arrow keys and press OK to confirm. The User management setup menu appears. In the "User management" setup menu, titrator users can be added or changed on a user list. The active user can be defined here; the user s access rights (Expert or Routine) can be changed. (See "5.8.4 Defining access rights") As long as no user is entered in the user list, the entry "No user" appears instead of the user name Adding a user - Press Setup to open the Setup menu. - Select "User management" using the arrow keys and press OK to confirm. The User management setup menu appears. - Select "User list" and press Modify. - Press Add. - Enter the name of the new user using the keypad and press Save to store the name you enter. METTLER TOLEDO DL15 45

48 Setup - The name appears in the user list. - You can quit the user list by pressing OK. - You can define another user by pressing Add Deleting a user - Press Setup to open the Setup menu. - Select "User management" using the arrow keys and press OK to confirm. The User management setup menu appears. - Select "User list" and press Modify. - Select the user who you want to delete from the list, and press Del. - The name is deleted from the user list Defining an active user - Press Setup to open the Setup menu. - Select "User management" using the arrow keys and press OK to confirm. The User management setup menu appears. - Select "Active" and press Modify. - The user list is displayed. - Select the user who you want to define as an active user from the list, and press Active to confirm your selection. - The new active user is displayed in the User management setup menu and on the Home screen. By pressing Inactive you can deactivate the active user. "No user" appears again on the display. 46 METTLER TOLEDO DL15

49 Setup Defining access rights The access rights for the user can be restricted through the setting "Routine". In this mode the user is only allowed to view and print settings in the Setup menu and methods and but cannot to change them. (Exeptions: Selection of the titration stand in the "Routine" mode and changing the active user.) Furthermore, in this mode it is not possible to delete results or statistics. - Press Setup to open the Setup menu. - Select "User management" using the arrow keys and press OK to confirm. The User management setup menu appears. - Select "Access". - By pressing Modify you can switch between the settings "Expert" and "Routine". - When you switch from "Expert" to "Routine", you will be requested to define a password. Enter a password using the keypad and press Save to store it in the titrator. - On switching from "Routine" to "Expert " you will be requested to enter the password you defined before. Enter the password using the keypad and press OK to confirm. - You can quit the setup menu for the user management by pressing OK. - The modified access rights are displayed on the Home screen. 5.9 Settings - Press Setup to open the Setup menu. - Select "Settings" using the arrow keys and press OK to confirm. The Settings setup menu appears. In this menu you can change different titrator settings such as date, time and language. The following settings can be made: Language Date Time Temperature unit Titrator ID Report header Beep METTLER TOLEDO DL15 47

50 Setup Setting the language You can choose German, English, French, Spanish, Italian and Russian. - Press Setup to open the Setup menu. - Select "Settings" using the arrow keys and press OK to confirm. The Settings setup menu appears. - Select "Language" and using Modify switch to your desired language. - Press OK to accept your changes and quit the menu, or press Esc to discard your changes and quit the menu Setting the date You can change the date stored in the titrator and the date format. - Press Setup to open the Setup menu. - Select "Settings" using the arrow keys and press OK to confirm. The Settings setup menu appears. - Select "Date". - Press Modify. - Select "Day", "Month" and "Year" one after the other and enter the current date using the keypad. - Select "Format" and press Modify to change to your desired date format. Four different date formats are available: /31/ Nov-2004 Nov/31/ Press OK to accept your changes and quit the menu, or press Esc to discard your changes and quit the menu. 48 METTLER TOLEDO DL15

51 Setup Setting the time - Press Setup to open the Setup menu. - Select "Settings" using the arrow keys and press OK to confirm. The Settings setup menu appears. - Select "Time". - Press Modify. - Select "Hour" and "Minute" one after the other and enter the current time. - Select "Format" and press Modify to change to your desired time format. Two different time formats are available: 05:00 pm 17:00 - Press OK to accept your changes and quit the menu, or press Esc to discard your changes and quit the menu Defining the temperature unit - Press Setup to open the Setup menu. - Select "Settings" using the arrow keys and press OK to confirm. The Settings setup menu appears. - Select "Temp. unit" and press Modify to change to your desired temperature unit. The temperature units available are: C, F and K. - Press OK to accept your changes and quit the menu, or press Esc to discard your changes and quit the menu Entering the titrator ID - Press Setup to open the Setup menu. - Select "Settings" using the arrow keys and press OK to confirm. The Settings setup menu appears. - Select "Titrator ID". - You can now enter any set of characters and numbers using the keypad. This ID is always included in the report. - Press OK to accept your changes and quit the menu, or press Esc to discard your changes and quit the menu. METTLER TOLEDO DL15 49

52 Setup Entering a report header - Press Setup to open the Setup menu. - Select "Settings" using the arrow keys and press OK to confirm. The Settings setup menu appears - Select "Report header" and press Modify. - You can now enter two lines of text using the keypad. These appear in the header of the report form. You can switch between the two text lines using the arrow keys. Each line can contain up to 24 characters. - Press OK to accept your changes and quit the menu, or press Esc to discard your changes and quit the menu Setting the beeper sound - Press Setup to open the Setup menu. - Select "Settings" using the arrow keys and press OK to confirm. The Settings setup menu appears - Select "Beep" and change to your desired setting using Modify. - There are two different settings for the beep sound: "No": A beep occurs only if there is a system malfunction. "Yes": A beep occurs each time a key is pressed, with system malfunctions, with error messages, and after performing a titration as soon as the results are displayed. - Press OK to accept your changes and quit the menu, or press Esc to discard your changes and quit the menu Titration stand - Press Setup to open the Setup menu. - Select "Titration Stand" using the arrow keys and press OK to confirm. The Titration Stand setup menu appears. In this menu you can select a titration stand and change between the internal overhead stirrer and the magnetic strirrer. - Select the menu item "Stand" with the arrow keys and press Modify to change to your desired setting "Internal", "Extern" or "Rondolino". "Internal": With this setting the titrator controls the internal titration stand. "Extern": The titrator can communicate with external devices (e.g. Kjeldahl distillation units of different manufacturers, pumps, etc.). See "13. Technical data". 50 METTLER TOLEDO DL15

53 Setup "Rondolino": Performing an automated sample series determination with a Rondolino sample changer requires this setting. - Select "Stirrer" using the arrow keys. - Press Modify to select "Magnetic stirrer" or "Overhead stirrer". If you select "Rondolino" as titration stand the setting "Overhead stirrer" is given. - Press OK to store your changes. METTLER TOLEDO DL15 51

54 Setup 52 METTLER TOLEDO DL15

55 Method 6. Methods (Method) Pressing the Method key opens the method editor. The titrator automatically performs analyses with the aid of predefined methods. In this chapter you learn how to open methods and how to define your own methods. A number of METTLER methods are already stored in the titrator. These methods have been developed by METTLER TOLEDO for certain applications and can be used directly for the corresponding analysis. See "6.7 Predefined methods". You can modify METTLER methods according to your requirements and store them as User methods. A complete titration method consists of sample preparation, stirring or waiting times, the actual titration itself, result calculation and a report. In the titrator, these steps are defined as functions. They are performed one after the other in an analysis. The individual functions consist of parameters whose values you can change. Method (Method ID / Name) Functions Parameter Sample Stir Measure EP titration Calculation 1 Calculation 2 Calculation 3 Report Parameter 1 Parameter 2 Parameter 1 Parameter 2 Parameter 1 Parameter 2 Parameter 1 Parameter 2 Parameter 1 Parameter 2 Parameter 1 Parameter 2 Parameter 1 Parameter 2 Parameter 1 Parameter 2 METTLER TOLEDO DL15 53

56 Method Each method has a name and a three-digit number that uniquely characterizes each method. For User methods, the method identification number (method ID) can be between 1 and 899. The range 900 to 999 is reserved for METTLER methods. You can create a new method by modifying the parameters of the functions of an existing method and storing them under a new method ID. The method editor can be opened by pressing the Method key. It allows you to create, modify, delete, print and start methods. 6.1 Starting a method There are three ways to start a method: - Using Run (see "8.1 Starting a sample determination using the Run key".) - Using the Home screen (Start of the three main methods, see "4.3.9 The Home screen"). - Using the method editor (see "6.1.1 Starting methods from the method editor") Starting methods from the method editor Proceed as follow to start a method from the method editor: - Press Method to open the method editor. - The Methods menu appears with the following items: Method ID User methods METTLER methods In the "Method ID" box, you can enter the method ID of an existing method (User or MET- TLER methods). - Press Start to execute the selected method. If you do not know the method ID of the method that you want to execute, you can use the arrow keys to select the method from a list using its name and method ID: - Select "User methods" if want to select a self-defined method. - Select "METTLER methods" if you want to select a METTLER TOLEDO predefined method. - Press OK to confirm. - In the display that follows, you can select the desired method from a list using its name and method ID. - Press Start to execute the selected method. 54 METTLER TOLEDO DL15

57 Method 6.2 Creating a method You can create a new method by changing the parameters of the functions of an existing method and storing the method under a new method ID. - Press Method to open the method editor. - The Methods menu appears with the following items: Method ID User methods METTLER methods - Select any method you want to modify and store as a new method. Selecting a method using its method ID You can enter the method ID of an existing method (User or METTLER method) in the "Method ID" box. - If you press Modify, the functions of the selected method are shown on the display. - Modify the individual functions according to your requirements. (See "6.3 Modifying a method") - Select "Title" and enter a title for the new method using the keypad. - Select "Method ID" and enter a method ID (range 1-899) for the new method. - Press OK. - A summary of the new method with method ID, title, author, date of creation and time appears on the display. - Press OK to store the new method. Selecting a method from the methods list If you do not know the method ID of the method you want to modify, you can use the arrow keys to select the method from a list using its name and method ID: - Select "User methods" if want to select a self-defined method. - Select "METTLER methods" if you want to select a predefined method from METTLER TOLEDO. - Press OK to confirm. METTLER TOLEDO DL15 55

58 Method - In the display that follows, you can use the arrow keys to select the desired method with its name and method ID from a list. - If you press Modify, the functions of the selected method are shown on the display. - Modify the individual functions according to your requirements. (See "6.3 Modifying a method") - Select "Title" and enter a title for the new method using the keypad. - Select "Method ID" and enter a method ID (range 1-899) for the new method. - Press OK. - A summary of the new method with method ID, title, author, date of creation and time appears on the display. - Press OK to store the new method. 6.3 Modifying a method You can modify the parameters of a User method as desired and afterward store the method again under its original method ID. If you want to modify the parameters of a METTLER method, you must afterward store the method as a User method under a new method ID. To modify the parameters of a method, you must first select the method: - Press Method to open the method editor. - The Methods menu appears with the following items: Method ID User methods METTLER methods - Select the method whose parameters you want to modify. Selecting a method using a method ID You can enter the method ID of an existing method (User or METTLER method) in the "Method ID" box. - If you press Modify, the functions of the selected method are shown on the display. - Modify the individual functions according to your requirements. - Press OK to store the new method. 56 METTLER TOLEDO DL15

59 Method Selecting a method from the methods list If you do not know the method ID of the method that you want to modify, you can use the arrow keys to select the method from a list using its name and method ID: - Select "User methods" if want to select a self-defined method. - Select "METTLER methods" if you want to select a predefined method from METTLER TOLEDO. - Press OK to confirm. - In the display that follows, you can select the desired method using its name and method ID from a list. - If you press Modify, the functions of the selected method are shown on the display. - Modify the individual functions according to your requirements. The parameters of the following functions are explained in the sections that follow: Sample Stirring Measuring EP titration Calculation Report METTLER TOLEDO DL15 57

60 Method Sample This function defines the request for sample information or the input of sample data such as weight, density and equivalent number, and temperature. The following parameters can be set: Request ID [Yes/No] This defines whether the ID of the sample is to be requested at the beginning of an analysis, "YES", or as a parameter in the method, "No". Select from the possible settings using Modify ID If "No" was selected, you can enter the sample ID here. The ID can be entered using the keypad. Entry type [Mass/Volume/Pieces] This defines whether the sample is to be added as defined mass, defined volume or a defined number of pieces. The request for sample data is then adapted with regard to units. Select from the possible settings using Modify Request sample [Yes/No] This determines whether mass, volume or number of pieces is to be requested at the beginning of the analysis or defined in the method. Select from the possible settings using Modify. Min. [ml] [g] [pcs.] This defines the lower limit for entry of the sample data at the start of the analysis. Appears only if "Yes" was selected for "Request sample". The unit depends on the setting of the parameter "Entry type". The desired value can be entered using the keypad. Max. [ml] [g] [pcs.] This defines the upper limit for the entry of the sample data at the start of the analysis. Appears only if "Yes" was selected for "Request sample". The unit depends on the setting of the parameter "Entry type". The desired value can be entered using the keypad. Weight [g] The weight of the sample. Appears only if "No" was selected for "Request sample" and "Mass" was selected as "Entry type". The desired value can be entered using the keypad. Volume [ml] The volume of the sample. Appears only if "No" was selected for "Request sample" and "Volume" was selected as "Entry type". The desired value can be entered using the keypad. 58 METTLER TOLEDO DL15

61 Method Density [g/ml] The density of the sample substance. Appears only if "No" was selected for "Request sample" and "Mass" or "Volume" was selected as "Entry type". The desired value can be entered using the keypad. Weight [g/pc.] The weight per piece of the sample substance. Appears only if "Number of pieces." as "Entry type" was selected. The desired value can be entered using the keypad. Number [pcs.] The number of sample units in a "piece". Appears only if "No" was selected for "Request sample" and "Number of pieces" as "Entry type" was selected. The desired value can be entered using the keypad. Mol.m. [g/mol] The molar mass of the sample substance in [g/mol] The desired value can be entered using the keypad. Equival. number z The equivalent number of the sample substance. The desired value can be entered using the keypad. Temp. Sensor [Manual/PT1000] Indicates whether the temperature is to be entered manually or determined automatically by the PT1000 temperature sensor. The temperature unit is the unit that was selected in the Setup. Select from the possible settings using Modify. Request [Yes/No] Indicates whether the temperature at the start of the analysis is to be requested or stored in the method. Appears only if "Manual" was selected for "Temp. sensor". Select from the possible settings using Modify. Temp. The temperature during the determination. Appears only if "Manual" was selected for "Temp. sensor" and "No" was selected for "Request temperature". The temperature unit is the unit that was selected in the Setup. The desired value can be entered using the keypad. METTLER TOLEDO DL15 59

62 Method Stir The parameters of the Stir function let you determine the speed of the overhead or magnetic stirrer during the analysis and whether the stirring time is to be requested before beginning the titration or defined in the method. Speed [%] The speed (rpm) of the stirrer during the analysis in %. (0%, stirrer does not rotate, 100%, stirrer rotates at the highest speed) The desired value can be entered using the keypad. Request duration [Yes/No] Indicates whether the stirring time is to be requested at the beginning of the analysis, "Yes", or is to be defined in the method, "No". The stirring time indicates how long the stirrer has to stir to homogenize the solution before the titration or the measurement is started. Select from the possible settings using Modify. Time [s] The stirring time. Appears only if "No" was set for "Request time". The stirring time indicates how long the stirrer has to stir to homogenize the solution before the titration or the measurement is started. The desired value can be entered using the keypad Measure The Measure function enables you to measure the potential of a solution under defined conditions. The following parameters can be set: Sensor Using Modify, you obtain the list of sensors from which you can select the desired sensor. Press OK to confirm. The unit (ph, or mv) is adapted for the other parameters according to the sensor selected. Unit [ph, px, mv] The unit for the measurement, depending on the sensor selected. You cannot change this parameter. Pol. Curr. [µa] The polarization current strength in [µa]. The desired value can be entered using the keypad. Appears only if you have selected a polarized sensor. 60 METTLER TOLEDO DL15

63 Method de[mv] The drift of the electrode potential must be less than de/dt during dt in order to be accepted as a measured value. This occurs during an interval defined by t(min) and t(max). The desired value can be entered using the keypad. dt[s] The drift of the electrode potential must be less than de/dt during dt, in order to be accepted as a measured value. This occurs during an interval defined by t(min) and t(max). The desired value can be entered using the keypad. t(min) [s] t(min) defines the earliest possible time that the measured value is accepted. The desired value can be entered using the keypad. t(max) [s] t(max) defines the latest possible time after which the measured value is in any case accepted. The desired value can be entered using the keypad EP titration Titr. Using Modify, you obtain the list of titrants from which you can select the desired titrant. Press OK to confirm. The concentration of the titrant from the Setup is used. Conc. [mol/l] The concentration of the titrant. You cannot change this parameter; the concentration of the titrant is used as defined in the Setup. Sensor Using Modify, you can access the list of sensors from which you can select the desired sensor. Press OK to confirm. The unit (ph, or mv) is adapted for the other parameters according to the sensor selected. px sensors are used like mv sensors in the method. The calibration parameters in the Setup are used to perform calculations for measured values in [ppm] or [mol/l] in the method. Unit [ph, mv] The unit for the measurement depending on the selected sensor. You cannot change these parameters. METTLER TOLEDO DL15 61

64 Method Pol. Curr. [µa] The polarization current strength in [µa]. The desired value can be entered using the keypad. Appears only if you have selected a polarized sensor. Blank [Entry/From list/request] Here you can define whether, at the beginning of the analysis, a blank value is to be requested, "Request"; entered in the method, "Entry"; or selected from the list of blank values, "From list". Select from the possible settings using Modify. Value [mmol] This parameter allows you to enter a blank value in the method. The desired value can be entered using the keypad. Appears only if "Entry" was selected for the parameter "Blank value". Solvent Using Modify, you obtain the list of blank values stored in the titrator. From there you can select a blank value and confirm by pressing OK. Appears only if "From list" was selected for the parameter "Blank value". Request predisp. [Yes/No] Here you can define whether a certain volume of titrant is to be predispensed before the start of the titration. With "Yes", this volume is requested before the beginning of the titration; with "No", you can enter the volume in the method. Select from the possible settings using Modify. Vol.[mL] With this parameter you can enter a volume for predispensing in [ml]. The desired value can be entered using the keypad. Appears only if "No" was selected for the parameter "Request predisp.". Req. back value [Yes/No] Here you can define whether a back value is to be requested at the beginning of the analysis, "Yes", or is entered in the method, "No". Select from the possible settings using Modify. Back val. [mmol] With this parameter you can define a back value in the method. The desired value can be entered using the keypad. Appears only if "No" was selected for the parameter "Req. back value" Control param. With the control parameters you can define the type of addition of titrant and the measure mode. You can access the parameters of this function using Modify. 62 METTLER TOLEDO DL15

65 Method Determin. [Normal/Cautious/Fast/User] Using the Determination parameter you can select a criterion for performing the titration. The possibilities are "Normal", "Cautious", "Fast" and "User". For the "Normal", "Fast" and "Cautious" settings, corresponding sets of parameters are stored in the titrator. You can view these parameters by printing the method. No other parameters need to be adapted. The "User" setting gives you the possibility to individually adapt all the parameters with regard to the addition of titrant and the measure mode. The following parameters "Addition" and "Measure" with the corresponding subparameters are only available if you have selected "User" for the parameter "Determination". Addition [Incremental/Dynamic] By using this parameter you can set whether the addition of the titrant is to be performed incrementally or dynamically. If you select "Incremental", the same volume increment is always added throughout the entire titration; if you select "Dynamic", the volume increment added during the titration is adapted dynamically within the preset limits to the course of the titration in order to obtain a constant potential difference per increment. Using Modify, you obtain the next screen on which you can select "Incremental" or "Dynamic" and define the subparameters using Modify. (For faster titrations, you should select "Incremental".) For the "Incremental" setting, the following parameters are available: dv [ml] Defines the size of the volume increment that is added in each dispensing step. This volume increment remains constant throughout the entire titration. The value in [ml] can be entered using the keypad. For the "Dynamic" setting the following parameters are available: denom [mv] Here you can enter the desired potential difference in [mv] per titration step. dvmin [ml] This value defines the minimum size of the volume increment. The value in [ml] can be entered using the keypad. dvmax [ml] This value defines the maximum size of the volume increment. The value in [ml] can be entered using the keypad. The range defined by dvmin and dvmax should be chosen as large as possible and the titrant addition controlled by denom. METTLER TOLEDO DL15 63

66 Method Measure [EQU controlled/fix time] You can select either equilibrium-controlled "EQU controlled" or timed increment "Fix time" measured value acquisition. Using these parameters, you can define the wait time until the measured value acquisition after an incremental addition. In the equilibrium-controlled measure mode the wait time is variable; in the timed increment mode it is constant. You can only decide which measure mode is best for your method when you know the reaction time of the components and the response time of the sensor used. Equilibrium measure mode is used for acid/base titrations in aqueous solutions, argentometric, complexometric, surfactant and redox titrations. Timed increment is used for acid/base titrations in nonaqueous solutions. Using Modify, you obtain the next screen where you can select "EQU controlled" or " Fix time" and define the subparameters using Modify. For the "EQU controlled" setting the following applies: Before the titrator dispenses the next increment, equilibrium must have been reached and the measured value must have stabilized. Responsible for the equilibrium is the measured change in potential, de, in the solution within the defined time dt. The wait time to the next incremental addition also depends on the definition of the minimum time (tmin) and the maximum time (tmax). As soon as the change in potential of the solution is less than the defined equilibrium (de/dt), the titrator accepts the measured value and adds the next increment. This can occur at the earliest at tmin and occurs at the latest at tmax. At tmax the measured value is in any case accepted even if the equilibrium condition is not met. This measure mode has the result that the incremental addition is fast in the flat part of the titration curve, and slow in the steep part. The following parameters are available: de [mv] Defines the maximum change in potential per time interval dt in [mv]. The desired value can be entered using the keypad. dt [s] Gives the time interval for the calculation of the calculation de[mv]/dt[s]. The desired value can be entered using the keypad. t(min) [s] Defines the wait time in [s] after which measured value acquisition occurs at the earliest. The desired value can be entered using the keypad. t(max) [s] Defines the wait time in [s] after which the measured value is in any case accepted. The desired value can be entered using the keypad. 64 METTLER TOLEDO DL15

67 Method For the "Fix time" setting the following applies: The titrator waits for the time interval defined by dt after each incremental addition before it adds the next increment. The following parameters are available: dt [s] Defines the wait time dt in [s] after each incremental addition. The desired value can be entered using the keypad. You can access the parameters of this function using Modify Recognition The Recognition function lets you set the tendency for endpoint recognition. You can access the parameters of this function using Modify. Tendency [Positive/Negative] Select "Positive" if you want the endpoint to be detected only for a positive tendency; select "Negative" if you want the endpoint to be detected only for a negative tendency. You can select from the possible settings using Modify. If the start potential already exceeds EP, the titration is terminated without the addition of titrant. For a relative EP the tendency describes the position of the EP related to the measured start potential Termination param. The termination parameters let you determine when a titration is terminated. You can access the parameters of this function using Modify. Vmax [ml] The maximum volume of titrant dispensed during the determination. This parameter is a safety measure to prevent unnecessary addition of titrant if a malfunction occurs during the titration. The desired value can be entered using the keypad. At tmax [Yes/No] This parameter lets you define whether the titration is to be terminated after a certain time, "Yes", or not "No". t(max) [s] This parameter lets you define the time interval after which the titration is terminated. The desired value can be entered using the keypad. This parameter appears only if "Yes" was selected for the parameter "At tmax". METTLER TOLEDO DL15 65

68 Method Evaluation The Evaluation function lets you define which endpoint of the titration is to be evaluated. You can access the parameters of this function using Modify. Numb. EPs [None/1/2] The number of potentials that are to be additionally evaluated. Possible values are none, 1 or 2. Select from the possible settings using Modify. End point 1 [Absolute/Relative] The type of endpoint determination for Endpoint 1. Absolute or relative to the start potential. Select from the possible settings using Modify. Appears only if "1" or "2" was selected for the parameter "Numb. EPs". Potential 1 [ph/mv] The value for Potential 1. The unit depends on the sensor used, ph or mv. The desired value can be entered using the keypad. Appears only if "1" or "2" was selected for the parameter "Numb. EPs". End point 2 [Absolute/Relative] The type of endpoint determination for Endpoint 2. Absolute or relative to the start potential. Select from the possible settings using Modify. Appears only if "2" was selected for the parameter "Numb. EPs". Potential 2 [ph/mv] The value for Potential 2. The unit depends on the sensor used, ph or mv. The desired value can be entered using the keypad. Appears only if "2" was selected for the parameter "Numb. EPs". 66 METTLER TOLEDO DL15

69 Method Calculation You can define three different calculations per analysis (Calculation 1-3). The following parameters are available for this: Calculation [None/Cont./Consump./Meas. val./user def./blank/titer] The type of calculation, depending on the desired result. Select from the possible settings using Modify. None Content Consumption Measured value User def. Blank value Titer No calculation is performed. The result of the calculation gives the content of the analysis. The result of the calculation gives the consumption. A measured value is produced. A user-defined formula for the calculation can be selected. The formula for the calculation can be adapted with a factor and a constant to obtain the result in the desired unit. The blank value relative to 2. or 3. EPs is calculated. The titer relative to 2. or 3. EPs is calculated. Type [Cont. w. Blank/Cont. back titr./cont.] The type of content determination. Content, content with blank value or content back titration can be selected and indicate whether the titration parameter back value or blank value is taken into account for the result. If you select "Content with blank value", the default formula R=Q*C/m is replaced with R=(Q-Bl)*C/m. If you select "Content back titration", the default formula R=Q*C/m is replaced with R=(Ba- Q)*C/m. Appears only if "Content" was selected for "Calculation". Select from the possible settings using Modify. It is not sufficient, under the function EP-Titration to request or enter a blank value or back value for it to be included in the calculation. In addition, you must set the parameter "Type" in the calculation function accordingly. Formula For user-defined calculations, you can select a formula to calculate the results. (See " Table of formulas for the calculation of results".) Select from the possible settings using Modify. This parameter only appears if you have selected "User def." for the parameter "Calculation". C For user-defined calculations, you can enter a constant to convert the results to the desired unit. The desired value can be entered using the keypad. This parameter only appears if you have selected "User def." for the parameter "Calculation". METTLER TOLEDO DL15 67

70 Method The constant C is only included in the calculation if C is also present in the calculation formula. Factor For user-defined calculations, you can enter a factor to recalculate the results. The desired value can be entered using the keypad. This parameter only appears if you have selected "User def." for the parameter "Calculation". Name For user-defined calculations, you can enter a name that appears later in the report. The desired name can be entered using the keypad. This parameter only appears if you have selected "User def." for the parameter "Calculation". Unit You can select the desired unit for the result. The possibilities depend on the parameter Calculation. Select from the possible settings using Modify. Calculation: Content Calculation: Consumption Calculation: Measured value Calculation: User-def. [g/l] [mg/l] [mol/l] [eq/l] [meq/l] [mg/g] [%] [ppm] [mol/kg] [mmol/kg] [mmol/g] [mmol/l] [ml] [mmol] [ppm] [mmol/l] [g/l] [mol/l] [mv] [ph] [px] Can be freely chosen, depends on the formula for the calculation of the results. For user-defined calculations, the unit can be entered using the keypad. Which EP The parameter indicates for which number EP the result is calculated. Does not appear for determinations of the type "Measurement". The following possibilities are available for EP: 1, 2, Start value Select from the possible settings using Modify. Decimal places You can enter the number of decimal places for the result of the calculation. The desired value can be entered using the keypad. Result limits [Yes/No] Select "Yes" if you want to enter the limits for the result, or "No" if you want the result calculated independent of limits. Select from the possible settings using Modify. 68 METTLER TOLEDO DL15

71 Method Minimum Enter the lower limit for the calculated result. Appears only if you have selected "Yes" for the "Result limits". The desired value can be entered using the keypad. Maximum Enter the upper limit for the calculated result. Appears only if you have selected "Yes" for the "Result limits". The desired value can be entered using the keypad. If the result of a titration is outside the defined result limits, the result is marked with an exclamation point and a message appears on the display. Statistics [Yes/No] This parameter lets you define whether the statistics of the analysis is included in the report, "Yes", or not, "No". Select from the possible settings using Modify. The following table summarizes the formulas on which the individual calculations are based. METTLER TOLEDO DL15 69

72 Method Table of formulas for the calculation of results Calculation: Titer Calculation: blank value Calculation: consumption Calculation: measured value Calculation: content default formula: R = Q*C/m Calculation: user. def. R = m/(veq*c*c) R = Q ml: R = VEQ mv: R = E %: C = M/(10*z) R = Q*C/m (default formula) Liquid standards: C = 1/(cst*z) Solid standards: C = M/(1000*z) mmol: R = Q Q = VEQ*c*t ph: zero point[ph] + E[mV]/slope[mV/pH] px: zero point[px] + E[mV]/slope[mV] mg/g: C = M/z g/l: C = M/z ppm: R = pw(-px)*1000 ppm: C = M*1000/z ml: R = VEQ mmol/l: R = pw(-px)*1000 mg/l: C = M*1000/z R = (Q-Bl)*C/m (default formula including the blank value) R = (Ba-Q)*C/m (default formula including the back value) mmol: R = Q Q = VEQ*c*t g/l: R = pw(-px) mol/l: C = 1/z mv: R = E mol/l: R = pw(-px) mol/kg:c = 1/z R = pw(-px)*1000 (mmol/l, ppm or other unit of measure, depending on the position of the zero point) mmol/g:c = 1/z mmol/l: C = 1000/z mmol/kg: C = 1000/z eq/l: C = 1 meq/l: C = 1000 R = (Q-Bl)*C/m (content with blank value) R = (Ba-Q)*C/m (content back titration) R = pw(-px) (mol/l, g/l or other unit of measure, depending on the position of the zero point) The following table summarizes the symbols used and their meaning: E Potential [mv, ph...] of the function measure Bl Blank value [mmol] T Temperature [ C, F, K] Ba Back value [mmol] R Calculated result c Nominal concentration of the titrant [mol/l] C Calculation constant c*t Actual concentration of the titrant [mol/l] VEQ ml consumption t Titer Q VEQ*c*t [mmol] z Equivalent number M Molar mass [g/mol] cst Concentration of the liquid standard [mol/l] 70 METTLER TOLEDO DL15

73 Method Report This function lets you determine whether a report is to be printed or not and defines the size of the report. You can define the following parameters: Output [Printer/None] Determines whether a report is to be printed "Printer", or not "None". Select the setting you want using Modify. Results [GLP/None/Short] Determines the size of the presentation of the results in the report. "GLP" Good Laboratory Practice - comprehensive. "None" No presentation of the results. "Short" Brief presentation of the results. Select the setting you want using Modify. Meas. val. table [Yes/No] Determines whether a measured value table is to be included as part of the report, "Yes", or not "No". Does not appear for measurements. Select the setting you want using Modify. E - V curve [Yes/No] Determines whether a titration curve (potential plotted against volume) is to be included in the report, [Yes], or not, [No]. Appears only for measurements Select the setting you want using Modify. de/dv curve [Yes/No] Determines whether the first derivative of the titration curve (potential plotted against volume) is to be included in the report, [Yes] or not, [No]. Appears only for measurements Select the setting you want using Modify. METTLER TOLEDO DL15 71

74 Method 6.4 Deleting methods You can only delete User methods. The METTLER methods stored in the titrator cannot be deleted. To delete a method, you must first select it: - Press Method to open the method editor. Selecting a method using the method ID You can enter the method ID of an existing User method in the Method ID box. - By pressing Modify you can display the functions of the selected method. - Using Del. you can delete the selected User method. - On the screen that follows, you must select "Yes" and then press OK to confirm deletion. - The method is deleted and you return to the start screen of the Methods menu. Selecting a method from the methods list If you do not know the method ID of the method that you want to delete, you can select the method from a list using its name and method ID: - Select "User methods". - Press OK to confirm - On the screen that follows, use the arrow keys to select the desired method from a list using its name and method ID. - By pressing Modify, you can display the functions of the selected method. - Using Del. you can delete the selected User method. - On the screen that follows, you must select "Yes" and then press OK to confirm deletion. - The method is deleted and you return to the start screen of the Methods menu. 72 METTLER TOLEDO DL15

75 Method 6.5 Printing a methods list Proceed as follows to print a list of all the User or METTLER methods stored in the titrator: - Press Method to open the method editor. - The Methods menu appears with the following items: Method ID User methods METTLER methods - Select "User methods" using the arrow keys if you want to print a list of User methods. - Select "METTLER methods" if you want to print a list of the METTLER TOLEDO predefined methods. - Press Print to print the list of the methods. - You must confirm the next screen by pressing OK before the print job is started. 6.6 Printing a method To print the parameters of a method, you must first select the desired method. - Press Method to open the method editor. Selecting a method using the method ID You can enter the method ID of an existing User method in the Method ID box (User method or METTLER method). - Press Print to print the parameters of the selected method. Selecting a method from the methods list If you do not know the Method ID of the method you want to delete, you can select the method from a list using its name and method ID: - Select "User methods" using the arrow keys if you want to select a self-defined method. - Select "METTLER methods" if you want to select one of the predefined METTLER TOLEDO methods. - Press OK to confirm your selection - On the screen that follows you can select the desired method using its name and method ID from a list. - Press Print to print the functions and parameters of the selected method on the printer. - You must confirm the next screen by pressing OK before the print job is started. METTLER TOLEDO DL15 73

76 Method 6.7 Predefined methods Method ID Title Samples Method type Control param. Sensor Titrant / Standard Result 920 Acid content EP acids e.g. HCl EP titration EP = ph 7.0 DG115 NaOH 0.1 mol/l / KHP HCl (%) M = ; z=1 921 Base content EP base e.g. NaOH EP titration EP = ph 7.0 DG115 HCl 0.1 mol/l / THAM NaOH (%) M = 40.00; z=1 926 ph measure measure DG115 measured value ph 74 METTLER TOLEDO DL15

77 Series 7. Series Pressing the Series key opens the Series menu. From this menu you can perform any type of series determination (sample, titer or blanc value). An Important prerequisite for performing an analysis with the titrator is that you have properly set up all the necessary resources in the setup menu (See "5 Setup") and that the methods you need are available. You can create or modify the methods using the method editor (See "6 Methods"). Furthermore you have the possibility to automatize your series determination by using a Rondolino sample changer. Up to nine samples can be analyzed automatically. It is required to choose Rondolino as titration stand if you use a Rondolino sample changer. (See 5.10 Titration stand ) 7.1 Starting a sample determination using the Series key - Press the Series key. - The message: Statistics memory: Memory is cleared is displayed. Confirm with Proceed. - Under "Determination", select either "Sample", "Titer" or "Blank value", depending on the type of determination you want to perform, using Modify. - Select "Method ID" using the arrow keys. - Press Modify. - Select "User methods" if you want to select a self-defined method. - Select "METTLER methods", if you want to select one of the METTLER TOLEDO predefined methods. - Press OK to confirm your selection. - In the display that follows you can select the desired method from a list using its name and its method ID. - Press OK to confirm your selection. - Select Number of samples using the arrow keys and enter the desired number of samples (min. 1; max. 9) using the keypad. - Press OK to confirm your selection. Depending on the settings of the selected method a list of the samples and their related parameters is displayed. - Select the sample using the arrow keys. - Press Modify. - Enter the value of the respective parameter. - Press OK to confirm your selection. - Press Start to perform the selected method (you can press Modify to select another method or press List to adept the number of the samples). - The analyses are performed according to the instructions given in the method used. You can enter the method ID of an existing method (User method or METTLER method) in the "Method ID" box and then confirm this by pressing Start. METTLER TOLEDO DL15 75

78 Series 7.2 Starting a titer determination using the Series key - Press the Series key. - The message: Statistics memory: Memory is cleared is displayed. Confirm with Proceed. - Under "Determination", select "Titer" using Modify. - Select "Method ID" using the arrow keys. - Press Modify. - In the menu that follows, select either User methods or METTLER methods and confirm your selection by pressing OK. - Select a method that uses the titrant whose titer you want to determine, and confirm your selection by pressing OK. - Select Number of samples using the arrow keys and enter the desired number of samples (min. 1; max. 9) using the keypad. - Press OK to confirm your selection. Depending on the settings of the selected method a list of the samples and their related parameters is displayed. - Select the sample using the arrow keys. - Press Modify. - Enter the value of the respective parameter. - Press OK to confirm your selection. - Press Start to start the titer determination. - The titer determination is performed according to the instructions given in the method. (See "6.3 Modifying a method") - A report is sent to the printer, depending on the settings defined in the method. - After the determination you can view the statistics of the current sample series by pressing Stat.. - If the titer is within the defined limits, you can accept the result of the titer determination (or the mean result if you have performed the titer determination several times) by pressing Save. - The date and time of the last titer determination are automatically updated. - Quit the display that follows by pressing Esc. in order to prevent the date and time being set to and 00: METTLER TOLEDO DL15

79 Series 7.3 Starting a blank value determination using the Series key - Press the Series key. - The message: Statistics memory: Memory is cleared is displayed. Confirm with Proceed. - Under "Determination", select "Blank value " using Modify. - Select "Method ID" using the arrow keys. - Press Modify. - In the menu that follows, select either User methods or METTLER methods, and confirm your selection by pressing OK. - Select a method that references the blank value that you want to determine and confirm your selection by pressing OK. - Select Number of samples using the arrow keys and enter the desired number of samples (min. 1; max. 9) using the keypad. - Press OK to confirm your selection. Depending on the settings of the selected method a list of the samples and their related parameters is displayed. - Press Start to start the blank value determination. - The blank value determination is performed according to the instructions given in the method. (See "6.3 Modifying a method") - A report is sent to the printer, depending on the settings defined in the method. - You can view the statistics of the current sample series by pressing Stat.. - If the blank value is within the defined limits, you can accept the result of the blank value determination (or the mean result if you have performed the blank value determination several times) by pressing Save. The date and time of the last blank value determination are automatically updated. - Quit the display that follows by pressing Esc. in order to prevent the date and time being set to and 00:00. METTLER TOLEDO DL15 77

80 Series 78 METTLER TOLEDO DL15

81 Run 8. Analysis (Run) Pressing the Run key opens the Analysis menu. From this menu, you can perform any type of determination (sample, titer or blank value determination). An Important prerequisite for performing an analysis with the titrator is that you have properly set up all the necessary resources in the setup menu (See "5 Setup") and that the methods you need are available. You can create or modify the methods using the method editor (See "6 Methods"). 8.1 Starting a sample determination using the Run key - Press the Run key. - Under "Determination", select either "Sample", "Titer" or "Blank value", depending on the type of determination you want to perform, using Modify. - Select "Method ID" using the arrow keys. - Press Modify. - Select "User methods" if you want to select a self-defined method. - Select "METTLER methods", if you want to select one of the METTLER TOLEDO predefined methods. - Press OK to confirm your selection. - In the display that follows you can select the desired method from a list using its name and its method ID. - Press OK to confirm your selection. - Press Start to perform the selected method (you can press Modify to select another method or press Series to open the Series menu). - The analysis is performed according to the instructions given in the method used. You can enter the method ID of an existing method (User method or METTLER method) in the "Method ID" box and then confirm this by pressing Start. You can facilitate starting the three most frequently used methods by defining them as main methods in the Setup menu. The method ID of these main methods then appear on the Home screen and can be started from there by pressing the corresponding function key. (See "5.7 Main methods".) METTLER TOLEDO DL15 79

82 Run 8.2 Starting a titer determination using the Run key - Press the Run key. - Under "Determination", select "Titer" using Modify. - Select "Method ID" using the arrow keys. - Press Modify. - In the menu that follows, select either User methods or METTLER methods and confirm your selection by pressing OK. - Select a method that uses the titrant whose titer you want to determine, and confirm your selection by pressing OK. - Press Start to start the titer determination. - The titer determination is performed according to the instructions given in the method. (See "6.3 Modifying a method") - A report is sent to the printer, depending on the settings defined in the method. - After the determination you can view the statistics of the current sample series by pressing Stat.. - If the titer is within the defined limits, you can accept the result of the titer determination (or the mean result if you have performed the titer determination several times) by pressing Save. - The date and time of the last titer determination are automatically updated. - Quit the display that follows by pressing Esc. in order to prevent the date and time being set to and 00: Starting a blank value determination using the Run key - Press the Run key. - Under "Determination", select "Blank value " using Modify. - Select "Method ID" using the arrow keys. - Press Modify. - In the menu that follows, select either User methods or METTLER methods, and confirm your selection by pressing OK. - Select a method that references the blank value that you want to determine and confirm your selection by pressing OK. - Press Start to start the blank value determination. - The blank value determination is performed according to the instructions given in the method. (See "6.3 Modifying a method") - A report is sent to the printer, depending on the settings defined in the method. 80 METTLER TOLEDO DL15

83 Run - You can view the statistics of the current sample series by pressing Stat.. - If the blank value is within the defined limits, you can accept the result of the blank value determination (or the mean result if you have performed the blank value determination several times) by pressing Save. The date and time of the last blank value determination are automatically updated. - Quit the display that follows by pressing Esc. in order to prevent the date and time being set to and 00:00. METTLER TOLEDO DL15 81

84 Run 82 METTLER TOLEDO DL15

85 Performing a titration 9. Performing a titration This chapter explains the general procedure for performing a titration method, using a simple acid-base titration as an example. The method for determining the acid content is stored as a METTLER method under the method ID 900 entitled "Acid Content EP". The purpose of the method is to determine the acid content of an aqueous solution using an endpoint titration. The following determination is performed: approx. 5 g of an HCl solution (conc. 0.1 mol/l) is titrated with NaOH (conc. 0.1 mol/l). 9.1 Preparations Make up solutions of hydrochloric acid and sodium hydroxide in the concentrations given above. The sodium hydroxide must be free of carbonate. Prepare the burette for the sodium hydroxide and attach it to the titrator (see "3.2.2 Installing the burette"). To protect the sodium hydroxide from CO 2, mount a drying tube on the burette holder of the NaOH bottle. Attach a titration beaker to the titration stand and insert the NaOH dispensing tube into one of the smaller openings of the titration head. Connect the stirrer to the appropriate connection, and check that the stirrer is correctly configured under the settings for the titration stand. (See "5.10 Titration stand") If you use an overhead stirrer, attach it to the titration stand. If you use a magnetic stirrer, make sure that the titration arm is swiveled in and that the titration beaker is positioned above the magnetic stirrer. Fill the burette (see next page). A printer and/or a balance can be optionally connected to the titrator. (See "5.4 Peripherals") METTLER TOLEDO DL15 83

86 Performing a titration Filling the burette (rinsing) - Press the Burette key. - The menu of the Burette auxiliary function menu appears. - Select "Rinse" using the arrow keys and press Start to start the rinsing process. - The screen displays "Rinse" during the rinsing process. - The piston of the burette is moved upward and the air is forced out. A small volume of sodium hydroxide solution is sucked in when the piston returns to its initial starting position. - The main menu of the Burette auxiliary function appears on the display again: - Repeat the rinsing process twice to make sure that the burette is completely filled and the tubing has been well rinsed. Press the Reset key. The start screen appears. 9.2 Performing titration method 920 Connect the ph electrode to the sensor input "mv /ph" at the back of the titrator using the Lemo cable, and insert it into one of the larger openings of the titration stand. Then remove the titration beaker and rinse the dispensing tube and the electrode with deionized water. (If you are using an overhead stirrer, rinse the overhead stirrer as well.) Fill a titration beaker with approx. 50 ml deionized water, pipette in approx. 5 g of the hydrochloric acid solution and attach the beaker to the titration head. Make sure that the dispensing tube of the burette is attached to the titration stand and is inserted in the titration beaker. - Press the Run key. 84 METTLER TOLEDO DL15

87 Performing a titration - The Analysis start menu appears. - If the ID of method 900 is not shown under "Method ID", select the entry using the arrow keys, and enter "900" using the keypad. - "Sample" must be selected under "Determination". If this is not the case, select "Determination" and change the setting to "Sample" using Modify. - Press Start. - The Request sample display appears. - Now enter the weight of the sample (for this example, approx. 5g) using the keypad. - If a balance is connected to the titrator and is configured in the Setup menu, you can also transfer the sample weight directly from the balance. - Press Balance in the Request sample display. - The sample weight determined by the balance is shown on the display. - Pressing OK transfers the weight from the balance for your analysis. - Press OK or the Run key to start the titration. METTLER TOLEDO DL15 85

88 Performing a titration - An appropriate message appears on the display while the burette is being filled. - After the burette has been filled, the sample is stirred for the duration of the mixing time to make sure the solution is homogeneous. The duration of the mixing time can be defined in the method. (See "6 Methods (Method)") - The titration begins. - During the determination, the following information is shown on the display: The volume already dispensed in [ml] The measured potential in [mv] The measured ph of the solution The signal symbolized by the varying black bar. The bar indicates the limit below which the measured value of the potential is accepted. - During the titration, you can display the titration curve (measured potential plotted against dispensed volume) using Graph. A line shows the zero point of the y-axis (0 mv/ ph 7). - You can return to the measured values display by pressing Values. - You can terminate the titration by pressing Abort. Values already measured are however not lost. - At the end of the titration, the result is shown on the display and at the same time the analysis report is sent to the printer. - If you confirm the result by pressing OK, the start screen of the Analysis menu appears. - As long as the printout of the report on the printer is still in progress, the message "Reporting" appears on the display; the titrator does not return to the start screen of the Analysis menu until the printout is finished. - If you perform the determination several times, you can display the statistical evaluation of your results by pressing Stat.. - You can view the result of your titration using the Results auxiliary function. (See "10.6 Results") 86 METTLER TOLEDO DL15

89 Performing a titration - If you have not set up a printer in Setup, an error message is given at the end of the analysis, which you must confirm by pressing Abort. - The result is then shown on the display. - If you have connected a printer, the following report is printed: ================================================================= METTLER TOLEDO DLXX SNR V1.00 ID :21 User Meyer ================================================================= EP titration : Method ID 920 Sample No :05 Sample ID HCl EP titration Method ID 920 Title Acid content EP :05 Author Meyer Titer Titrant NaOH 0.1 Sensor DG115 Conz. [mol/l] 0.1 Unit ph Sample 1 Sample ID HCl Entry type Mass Mass [g] Minimum [g] 1.2 Maximum [g] 6.5 Density [g/ml] 1.0 Mol.m. [g/mol] Equival. number z 1 Predis. [ml] Mixing time [s] 3 Init.pot. [mv] Consumption [ml] Duration [min:s] 2:00 Temp. [ C] 25.0 Abort All points reached 0.00 Blank [mmol] Back value [mmol] 0.00 EP Volume [ml] Potential [ph] Result EP Calculat. Value Unit Cont [%] Statistics report Result n x s Unit srel [%] 0.00 [%] :21 Page :21 Page 2 METTLER TOLEDO DL15 87

90 Performing a titration 88 METTLER TOLEDO DL15

91 Auxiliary functions (Info, Sensor, Stirrer, Burette, Report, Results) 10. Auxiliary functions (Info, Sensor, Stirrer, Burette, Report, Results) The pictogram keys for the auxiliary functions enable you to open different titrator functions that are not involved in performing the actual analysis, but which can support or extend it. The auxiliary function keys are locked during an analysis that is running and the corresponding menus cannot be opened Information menu You can open the Info menu by pressing the pictogram key i. The following functions can then be opened: System information This function lets you view the system information for the titrator. System test This function lets you test the titrator hardware and any connected peripheral instruments, such as a balance or a printer. (See "11.2 Hardware tests") Service (This menu can only be accessed by service specialists.) 10.2 Sensor If you press the Sensor key, the list of sensors stored in the titrator appears. From this menu you can now select a sensor and with a temperature sensor, measure the temperature of a solution; with a ph, mv, ISE or polarized sensor, measure the potential of a solution; for a ph, or ISE sensor, perform a sensor calibration; for a ph, or ISE sensor, perform a sensor test. METTLER TOLEDO DL15 89

92 Auxiliary functions (Info, Sensor, Stirrer, Burette, Report, Results) Measuring temperature To measure the temperature of a solution: - Press the Sensor key. - Select "PT1000" for the temperature sensor using the arrow keys, and press Modify. - Press Start to start the measurement. - The measured signal is shown on the display. - You can terminate the measurement by pressing Stop. You can also start the measurement directly by pressing Start after selecting the temperature sensor. The setting last used is used for the stirrer speed. You can change the temperature unit in the "Settings" setup menu. (See "5.9.4 Defining the temperature unit") Measuring potential You can measure the potential of a solution using the appropriate sensors in mv, ph, or px: - Press the Sensor key. - Select the desired sensor for the measurements using the arrow keys and press Modify. - For polarized sensors, select "Pol. current [µa]" and enter the polarization current in [µa]. - Select "Speed [%]" and enter the desired speed for the stirrer in [%]. - For ph and px sensors, select "Temp. sensor" and using Modify select either "Manual" for manual temperature entry or "PT1000" for the measurement of temperature using a temperature sensor. - If you have selected manual temperature entry, for ph and px sensors enter the temperature in the given unit under "Temperature". - Press Start to perform the measurement. 90 METTLER TOLEDO DL15

93 Auxiliary functions (Info, Sensor, Stirrer, Burette, Report, Results) You can also start the measurement by pressing Start directly after selecting the sensor without changing the settings beforehand with Modify. The settings last used are then adopted Calibrating a sensor To perform a sensor calibration for a ph or ISE sensor: - Press the Sensor key. - Select the sensor you want to calibrate using the arrow keys. - Press Modify. - Press Calib. The calibration is performed in the same way as described in the setup section for sensor calibration from the setup menu. (See "5.3.5 Sensor calibration from the sensor setup menu") Testing a sensor To perform a sensor test for a ph or ISE sensor: - Press the Sensor key. - Select the sensor you want to calibrate using the arrow keys. - Press Modify. - Press Test. The sensor test is performed in the same way as described in the setup section for sensor calibration from the setup menu. (See "5.3.6 Sensor test from the sensor setup menu") 10.3 Stirrer If you press the Stirrer key, the Stirrer menu appears. This menu lets you switch a stirrer on and off (an overhead or a magnetic stirrer) and change its speed: - Press the Stirrer key to open the Stirrer menu. - Select "Speed [%]" and enter the desired stirrer speed in [%]. - Press Start to switch on the stirrer. - Press Stop to switch off the stirrer. METTLER TOLEDO DL15 91

94 Auxiliary functions (Info, Sensor, Stirrer, Burette, Report, Results) The Stirrer auxiliary function always refers to the stirrer that was selected in the "Titration stand" setup menu. To change from an overhead stirrer to a magnetic stirrer, you must make the corresponding settings in the setup menu. (See "5.10 Titration stand") 10.4 Burette If you press the Burette key, the Burette auxiliary functions menu appears. You can select and execute the following functions: Rinse the burette. Rinse the tip of the burette. Dispense a defined volume. Perform a manual titration Rinsing the burette - Press Burette to open the burette auxiliary functions. - "Rinse" is already selected. - Press Modify to change the settings for the rinsing process. - Select "Fill rate [%]" to change the speed at which the burette is filled. Enter a value for the fill rate. - Select "No. of rinse cycles" and enter how many times you want to empty and fill the burette. - Press Start to start the rinsing process. The titrator completely empties and fills the burette each cycle. The piston of the burette is moved to below its zero position so that air bubbles possibly present around the stopcock are also removed. A lower fill rate is recommended for reagents of high viscosity in order to prevent air being sucked in. Make sure in rinsing processes that the waste container under the dispensing tube is sufficiently large. You can also start the rinsing process at the rinsing rate shown by selecting "Rinse" and pressing Start. 92 METTLER TOLEDO DL15

95 Auxiliary functions (Info, Sensor, Stirrer, Burette, Report, Results) Rinsing the tip - Press Burette to open the Burette auxiliary functions. - Select the parameter "Rinse tip" using the arrow keys. - Press Start to start the rinsing process. - 5% of the burette volume is dispensed to remove possible contaminants from the tip of the dispensing tube. Make sure during the rinsing processes that the waste container under the dispensing tube is sufficiently large Dispensing - Press Burette to open the Burette auxiliary functions. - Select "Dispense" using the arrow keys. - Press Modify to change the settings for the dispensing process. - Under "Volume", enter the volume in [ml] that you want to dispense. - Select "Burette", and using Modify, select the volume of the burette you are using (1 ml, 5 ml, 10 ml or 20 ml). - Select "Fill rate [%]" to change the speed at which the burette is filled. Enter a value for the fill rate. - Press Start to start the rinsing process. A lower fill rate is recommended for reagents of high viscosity in order to prevent air being sucked in. You can also start the dispensing process by selecting "Dispense" and pressing Start. The settings last used are adopted for the fill rate and the burette volume Manual titration - Press Setup to open the setup menu. - Select "Titrants" using the arrow keys and press OK to confirm. The list of the titrants stored in the titrator appears. - Select the titrant and press Modify. - Confirm the selection with Save. - Press Esc to change to the setup menu. - Select "Sensors" using the arrow keys and press OK to confirm. The list of the sensors stored in the titrator appears. - Select the desired sensor and press Modify. - Confirm the selection with Save. - Press Burette to open the Burette auxiliary functions menu. METTLER TOLEDO DL15 93

96 Auxiliary functions (Info, Sensor, Stirrer, Burette, Report, Results) - Select "Man. Titration" using the arrow keys. - Press Start to perform a manual titration. - By pressing the numeric input keys (0 to 9) you define the volume of the increment you want to dispens. The volume of the manual dispensed increments depends both on the volume of the burette used and the numeric key. Press "1" to dispens the lowest volume depending on the burette used up to "0" to dispens the highest volume. The following table displays the volume of increments in ml for different burette sizes. Key Increment [ml] 1 ml burette Increment [ml] 5 ml burette Increment [ml] 10 ml burette Increment [ml] 20 ml burette *) *) *) *) *) Rounded values are indicated. (Three decimal places) A continuous titration can be performed by permanently pressing a numeric key. However it is not possible to dispense a defined volume. Therefore a manual titration is conditionally recommendable. 94 METTLER TOLEDO DL15

97 Auxiliary functions (Info, Sensor, Stirrer, Burette, Report, Results) 10.5 Report If you press the Report key, Report auxiliary functions menu appears. This enables you to print additional reports of the determination or measurement you performed last. - Press Report to open the Report menu. - Using the arrow keys, select "Results" and with Modify select either "Short" or "GLP". (GLP stands for "Good Laboratory Practice" and means the maximum possible detail of the results) - Using the arrow keys, select "Meas. val. table" and with Modify select "Yes" or "No", depending on whether the report should contain the measured results in table form or not. - Using the arrow keys, select "E-V curve" and with Modify select "Yes" or "No", depending on whether the report should contain a titration curve (measured potential plotted against consumed volume) or not. - Using the arrow keys, select "de/dv curve" and with Modify select "Yes" or "No", depending on whether the report should contain the 1st derivative of the titration as a curve or not. If no analyses or measurement results are stored in the titrator, only the message "No results" appears on opening the Report menu and you cannot perform any settings in this menu. "Meas. val. table", "E-V curve" and "de/dv curve" are not available for reports of measurements Results Pressing Results leads you into the menu of the Results auxiliary function. This function enables you to view and print the results of a series of determinations or measurements; view and modify the statistics of a series of determinations or measurements; terminate a series of determinations or measurements. If no analyses or measurement results are stored in the titrator, only the message "No results" appears on opening the Results menu and you cannot perform any settings in this menu. METTLER TOLEDO DL15 95

98 Auxiliary functions (Info, Sensor, Stirrer, Burette, Report, Results) Displaying and printing results - Press Results. - Select "All results" using the arrow keys and confirm with OK. - In the menu that follows, under "Number of samples" you can select the number of results stored in the titrator", and under "Method", the method used for the current sample series. - Select "Results samp. no." and enter the sample number of the sample whose result you want to view or print. - Press Print to print the result. - Press Show to present the result on the display. If no analyses or measurement results are stored in the titrator, the message "No results" appears on opening the Results menu, and you can not perform any settings in this menu. To select an individual result from a list of all the stored results, select "Number of samples" and press List. You can then select any result using its sample number, and view it by pressing Show. To print the method with which the sample series was performed, select "Method" and press Print. While the results are shown on the display, you can view the following or the previous results using Next and Back Statistics In the Statistics menu you can view and print a statistical evaluation of the results of your current sample series. A sample series is always a series of analyses with the same (unchanged) method. It does not matter whether the analyses consist of a series of blank value determinations, titer determinations, or sample determinations. You can exclude individual samples from the statistical evaluation by deleting them from the statistics memory. You can still view deleted samples in a list of the deleted results and return them to the statistics if desired. 96 METTLER TOLEDO DL15

99 Auxiliary functions (Info, Sensor, Stirrer, Burette, Report, Results) Displaying or printing a sample series - Press Results to open the Results menu. - Select "Statistics" using the arrow keys and press OK to confirm. - The statistics of the current sample series are shown on the display. - For each calculation defined in the method used (R1 to R3), the display shows the number of results (n) used for the statistics, the mean value of the calculation results (x), the standard deviation (s), and the relative standard deviation (srel). - Press Print to print the statistics. - In the menu that follows you can define whether or not the statistics are to be printed with the individual results. - Select "With results" and using Modify, set "Yes" or "No". - Press Start to start the print task. - For blank values and titer determinations, you can transfer the mean value of the determinations performed into the setup using Save. Removing results from the statistics - Press Results to open the Results menu. - Select "Statistics" using the arrow keys and press OK to confirm. - The statistics of the current sample series are shown on the display. - Press Modify to make changes to the statistics. - Select "Active samples" and press List. - In the list of active samples that follows, you can select the desired result and view it using Show. - If you press Del., the result displayed is deleted from the statistical evaluation and stored under "Deleted samples". - If you press Next and Back you can view the next or the previous result on the list and if necessary remove it from the statistics using Del.. To select an individual result using its sample number, select "Results samp. no." and enter the sample number using the keypad. You can view the result by pressing Show and then if necessary remove it from the statistics using Del.. METTLER TOLEDO DL15 97

100 Auxiliary functions (Info, Sensor, Stirrer, Burette, Report, Results) Adding a result to the statistics - Press Results to open the Results menu. - Select "Statistics" using the arrow keys and confirm with OK. - The statistics of the current sample series are shown on the display. - Press Modify to make changes to the statistics. - Select "Deleted samples" and press List. - In the list of deleted samples that follows, you can select the desired result and view it by pressing Show. - If you press Add, the result displayed is added to the statistical evaluation and removed from under "Deleted samples". - If you press Next and Back, you can view the next or the previous result on the list and if necessary return it to the statistics by pressing Add. To select an individual result using its sample number, select "Results samp. no." and enter the sample number using the keyboard. You can view the result by pressing Show and then if necessary add it to the statistics with Add Terminating the series The "Terminate series" menu enables you to terminate the current sample series. All the results stored in the titrator and the statistics memory are deleted. - Press Results to open the Results menu. - Select "Terminate series" using the arrow keys and confirm with OK. - Answer the following question "End series?" with "Yes". - The results of the current sample series and statistics memory are now deleted. If no analyses or measurement results are stored in the titrator, the message No results" appears on opening the Results menu and you can not perform any settings in this menu. 98 METTLER TOLEDO DL15

101 Error messages, malfunctions and hardware tests 11. Error messages, malfunctions and hardware tests 11.1 Global errors and malfunctions The following is summary of errors and malfunctions that the titrator does not display. In many cases it may help you to rectify a problem yourself without assistance from METTLER TOLEDO Service (in the table written as "Service"). Some malfunctions can be investigated using the hardware test (see Section 11.2) before you contact Service. Error Possible cause Action to be taken No display on the titrator. Several points of the display are missing. The display and the keys pressed do not match. Transfer error to attached peripheral. Instrument (printer, balance) does not react. TTL inputs or outputs are not functioning properly. Burette and stopcock do not go to the zero position on switching on. Magnetic stirrer bar does not turn. Titrator is not connected to the power supply. Device is faulty or switched off. Instrument is not switched on; wrong settings and/or configuration (switch settings wrong); wrong cable. Inputs and/or outputs are faulty. Burette drive faulty. Cable of the magnetic stirrer is not properly plugged in; wrong magnetic stirrer bar. Connect to power supply, otherwise contact Service. Contact Service. Contact Service. Check whether the attached device is functioning properly. Switch on instrument; settings and configuration must match. Check inputs/outputs. Contact Service. Check magnetic stirrer; replace magnetic stirrer; use the stirrer bar supplied. Wrong potential values. Electrode is faulty or dirty. Check electrode (see electrode data sheet) or use new electrode. No dispensing, titrant is discharged from stopcock or piston. Burette tip is blocked. Clean burette tip. METTLER TOLEDO DL15 99

102 Error messages, malfunctions and hardware tests 11.2 Hardware tests The System test menu includes different functions to test the titrator hardware and any connected peripheral instruments such as a balance or a printer. Proceed as follows to open the System test menu: - Press i to open the Info menu i. - Select "System test" using the arrow keys and then press OK to confirm. - You can now open the User interface, Comm. interface, Auxiliary I/O and ph input menus User interface - Press i to open the Info menu. - Select "System test" using the arrow keys and press OK to confirm. - Select "User interface" and press OK to confirm. You can now select and open the following functions by using the arrow keys and pressing OK. Screen test The screen alternately shows a full and then an empty display. This enables you to identify faulty pixels on the display. The test mode automatically switches off after about 10 seconds. Keypad test As soon as you press a key, a number code assigned to this key appears so that you can identify a faulty key (see following table). - You can quit the keypad test by pressing Esc. Key codes KeyCode Key Code Key Code Reset 101 Run i 105 F Stirrer 116 F Report 112 F Sensor Burette 98 Δ Results 117 Shift Setup Del 8 Method Series METTLER TOLEDO DL15

103 Error messages, malfunctions and hardware tests Beeper test You can check the internal beeper: press Start to switch it on, and Stop to switch it off Communication interfaces - Press i to open the Information menu i. - Select "System test" using the arrow keys and then press OK to confirm. - Select "Comm. interface" and then press OK to confirm. You can now select and open the following functions by using the arrow keys and pressing OK. Interface test To test the RS-232C interfaces, you must plug the test connector into the balance or RS-P42-interface. To test the Centronics interface, you must plug the Centronics cable into the Centronics interface and plug the test plug into the Centronics socket of the cable. - Then select the interface you want to test using the arrow keys and press Start. - After the test, the message "Test successful" or "Test failed" appears on the display. - Press OK to return to the menu. Printer test (GA42, RS-P42, HP) The printer must be connected. If the error message "Printer: no connection" appears, press Esc to cancel the error message - If you press "OK", the titrator again tries to establish communications with the printer. - After the test, the message "Test successful" or "Test failed" appears on the display. - If the test was successful, the letters and characters available in the titrator are printed. METTLER TOLEDO DL15 101

104 Error messages, malfunctions and hardware tests Balance test To perform the balance test, a weight must first be placed on the balance. When you press Start, the weight shown on the balance must appear on the titrator display Auxiliary I/O - Press i to open the Information menu i. - Select "System test" using the arrow keys and then press OK to confirm. - Select "Auxiliary I/O" and then press OK to confirm. You can now select the following functions using the arrow keys and open them by pressing OK. TTL-I/O - Before starting the test, plug the test plug into the TTL-I/O interface. After the test, the message "Test successful" or "Test failed" appears on the display. Overhead stirrer This test allows you to check whether the overhead stirrer operates properly at different speeds. - Select "Overhead stirrer" using the arrow keys and then press OK to confirm. - On the display that follows, you can enter a speed and switch on the overhead stirrer by pressing Start. - Press Stop to switch off the stirrer again. Magnetic stirrer This test allows you to check whether the magnetic stirrer operates properly at different speeds. - Select "Magnetic stirrer" using the arrow keys and then press OK to confirm. - On the display that follows, you can enter a speed and switch on the magnetic stirrer by pressing Start. - Press Stop to switch off the stirrer again. 102 METTLER TOLEDO DL15

105 Error messages, malfunctions and hardware tests ph input value This test allows you to check whether the ph input of the titrator is properly adjusted. - Select "ph input" using the arrow keys and then press OK to confirm. - You are requested to apply a voltage of 0 mv at the input for the mv/ph electrode. - Press OK to continue the test. - A value of ± 5% must appear on the display. - Press OK. - A value of 0.00 mv must be displayed. METTLER TOLEDO DL15 103

106 Error messages, malfunctions and hardware tests 104 METTLER TOLEDO DL15

107 Optional accessories and maintenance 12. Optional accessories and maintenance 12.1 Optional accessories HP-compatible printer on request Connection cable for METTLER TO- LEDO balance AE with option Printer RS-P42 Connection cable for SARTORIUS balances Connection cable for RS-P42 printer Connection cable for METTLER TOLEDO balances AG, AB, PB, PG (LC interface) Phototrode (incl. power supply unit) for color-indicated titrations Transmission measurement at 555, 660, 520, 620, 590 nm DP5 Adapter cable (DIN-LEMO) for attachment of electrodes or phototrode with DIN connector to the titrator Pt1000 temperature sensor DT1000 Connection cable for METTLER TOLEDO balances AM, PM, AT Triaxial cable SC-LEMO (Length: 60 cm) (Length: 100 cm) (Length: 160 cm) Compact stirrer LEMO cable connector (4 pin) for temperature sensors (non-mettler TOLEDO) Propeller stirrer (2x) Connection cable for METTLER TO- LEDO balances AB, AX, PB, PG-S (RS9 interface) Interchangeable burette 1 ml DV ml DV ml DV ml DV1020 METTLER TOLEDO DL15 105

108 Optional accessories and maintenance Connection cable between DL15/ DL22F&B/DL28, T50/T70/T90 titrator and Rondolino (Cable included in Rondolino delivery.) Sensors DG101-SC Combined ph electrode for small volumes in small titration vessels in aqueous solutions DG111-SC Combined ph electrode for titrations in aqueous solutions DG113-SC Combined glass electrode with movable sleeve frit for titrations in nonaqueous solutions DG114-SC Combined glass electrode with movable sleeve for titrations in aqueous solutions Ion selective electrodes Fluoride ISE DX219 Potassium ISE DX239 Calcium ISE DX240 Chloride ISE DX235 Nitrate ISE DX262 Ammonium ISE DX218 Bromide ISE DX280 DM140-SC Combined platinum ring electrode for redox titrations DM141-SC Combined silver ring electrode for argentometric titrations DM143-SC Double-pin platinum electrode 106 METTLER TOLEDO DL15

109 Optional accessories and maintenance 12.2 Service and maintenance Cleaning - The housing of the titrator can be cleaned with a cloth moistened with alcohol. - To clean the titration stand you can disassemble it into its parts and clean these individually (See Attaching the titration stand to the titrator) Disposal In conformance with the European Directive 2002/96/ EC on Waste Electrical and Electronic Equipment (WEEE) this device may not be disposed of in domestic waste. This also applies to countries outside the EU, per their specific requirements. Please dispose of this product in accordance with local regulations at the collecting point specified for electrical and electronic equipment. If you have any questions, please contact the responsible authority or the distributor from which you purchased this device. Should this device be passed on to other parties (for private or professional use), the content of this regulation must also be related. Thank you for your contribution to environmental protection. METTLER TOLEDO DL15 107

110 Optional accessories and maintenance 108 METTLER TOLEDO DL15

111 Technical data 13. Technical data Power supply Voltage range VAC ±10% Frequency 50/60 Hz Power consumption 45 VA Output voltage 24 VDC 0.8 A / 5 VDC 1.2 A Dimensions Width 240 mm Depth 305 mm Height 370 mm Weight approx. 5 kg Materials Titrator housing polypropylene Titration stand polypropylene Keyboard housing polyester Keyboard film polyester Spacing ring polypropylene Clamping ring polypropylene Threaded ring polypropylene Ambient conditions Ambient temperature +5 C to +40 C Atmospheric humidity max. 80% at 40 C Use Use indoors Overvoltage category II Pollution degree 2 ph/mv input Triaxial socket Range mv Resolution 0.1 mv Max. permissible error 2 mv Input resistance >10 12 Ω Polarized input Triaxial socket Pol. current µa Resolution 0.1 µa Max. permissible error 0.3 µa Measurement range mv Resolution 0.1 mv Max. permissible error 2 mv Pt pin socket (Lemo) Measurement range C Resolution 0.1 C Max. permissible error 0.2 C Magnetic stirrer output 8-pole socket (mini DIN) Motor stepper motor (AC) Speed software-controlled (1-100%) Power consumption 2 W Max. speed 1050 rpm (at 70%) Overhead stirrer output 5-pole socket (mini DIN) Motor DC motor Speed software-controlled (1-100%) Voltage range 0 to 18 V DC (max. 300 ma) METTLER TOLEDO DL15 109

112 Technical data Burette drive Drive Stepper motor Resolution 1/10000 of the burette volume Max. permissible error At 10% 15 µm At 30% 15 µm At 50% 25 µm At100% 50 µm Filling time minimum 20 s (rate can be set between 10 and 100%) Discharge time minimum 20 s Interchangeable burettes Volume 1, 5, 10 und 20 ml Max. permissible error Acc. to ISO (2002) (drive and burette) Materials that come into contact fluoroplastic, borosilicate glass, ceramics with the titrant Magnetic stirrerr Type Stepper motor Max. speed 1050 rpm Power consumption 2 W Overhead stirrer Type DC motor Max. speed 3800 rpm Power consumption 6 W Display LCD 6 lines, backlit Languages German, English, French, Spanish, Italian, Russian User data memory User methods max. 30 Titrants max. 30 Standards max. 20 Blank values max. 20 Sensors max. 20 RS-P42 Interface Baud rate 1200 baud Parity no Data bit 8 Stop bit 2 Handshake off Connection possibilities for peripheral instruments Balance Printer Connection by means of RS232C interface (9-pin D-Sub plug) for METTLER TOLEDO and SARTORIUS balances. Connection by means of RS232C interface (9-pin D-Sub plug) for RS-P42 und GA 42 printers. Connection by means of Centronics interface (25 pin D-Sub socket) for HP compatible printers with parallel interface. 110 METTLER TOLEDO DL15

113 Technical data RS232C connector (balance/ga42/computer) RxD (In) TxD (Out) DTR +12 V GND Data to titrator Data from titrator Handshake from titrator ready for operation Signal ground, galvanically coupled to titrator electronics TTL I/O socket IN1 IN2 OUT1 OUT2 OUT3 OUT4 GND In Out GND TTL; short circuit proof; pulse 150 ms (the input signal must be at least 150 ms for the titrator) Open collector Vce max. = 24 V Ic max. = 20 ma Signal ground, galvanically coupled to titrator electronics Centronics socket \Strobe PD0 PD1 PD2 PD3 PD4 PD5 PD6 PD7 \ACK \BUSY PE SLCT \AUTOFDXT \ERROR \INIT \SLCTIN Data ready Data transferred Printer busy End of paper Printer active Printer error Automatic line feed Printer initializing printer selected Signal ground, galvanically connected to titrator electronics METTLER TOLEDO DL15 111

114 Technical data TTL interface description 1. Basics The TTL interface of the titrator is used to communicate with external devices via several signals. Not only the Rondolino sample changer can be controlled by using the interface but also several third party devices ( e.g. Kjeldahl distillation units, pumps, etc.) 2. Hardware The interface consists of 4 output lines (Out1, Out2, Out3, Out4) and 2 inputs (In1, In2). They are provided on a 9 pin D-Sub connector using the following scheme: Signal In1 In2 Out1 Out2 Out3 Out4 Ground Pin Functionality 3.1 Signals providing sample handling Out2 This signal is activated on initializing a titration. Its rests active until return to the home state. On handling a sample series using Rondolino a follwing sample must be initialized within 1 second, otherwise Rondolino returns to ist home position (beaker 0). The signal Out2 is always set, irrespective of the selected titration stand setting Out4 An active pulse of about 200ms on Out4 after initialization of a titration indicates a request of a ready signal on In1. On handling a series using a Rondolino this pulse raises about 600ms after activation of Out2, otherwise it raises after input of the sample data is done by the user. The signal Out4 will only be activated if selection of titration stand setting ist Rondolino or External In1 After the pulse on Out4 has raised, the titrator expects the activation of signal In1. This will be done by Rondolino or an external titration stand, declaring the sample is now ready to be analyzed. Using Rondolino this means the beaker is reached an dipped in. In1 rests active till a following activation on Out1. The signal In1 will only be expected if selection of titration stand setting ist Rondolino or External Out1 The start of the titation in the inner sense is indicated by a pulse of 200ms on Out1. At this time the stirrer will be started an the mixing time starts counting down. The signal Out2 is always set, regardless of the selected titration stand setting. 112 METTLER TOLEDO DL15

115 Technical data Illustrations The following illustration shows the above described sequence of signals handling a Rondolino series of 3 samples. The following illustration shows some details of the one above. On the left side it can be seen, that 600ms after activa-tion of Out2 a pulse of 200ms raises on Out4, by which Rondolino starts moving to the next position. The arrival of this position is indicated after about 8s by activating In1. By this the titrator is stimulated to start titration and to raise a pulse on Out 1. Seeing this pulse on Out1 Rondolino deactivates In1. METTLER TOLEDO DL15 113