KF Titrators DL31 / DL38

Transcription

1 Operating Instructions KF Titrators DL31 / DL38

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3 Contents Page 1 The DL31/DL38 KF titrators Safety measures Measures for your protection Measures for operational safety The titrator Putting into operation The operating concept The command keys The menu keys The auxiliary function keys The <i> key The entry and arrow keys Changing the language Setup (<Setup> key) KF titrants Br No. titrants (DL38 only) KF standards Main methods (DL38 only) Peripherals Printer Balance Titration stand Computer Settings Methods (<Method> key) The KF standard method KF method parameters No. (of the method) Title (of the method) Sample parameters Speed Mix time Titrant Volume (for predispensing) Wait time (after predispensing) Auto start (DL38 only) Control parameters Termination parameters Blank Drift METTLER TOLEDO DL31/DL38 1

4 Result (DL31 only) Calculation (DL38 only) Standby Report Author of the method Storage procedures User and METTLER methods (DL38 only) METTLER methods "908 Bromine No." and "909 Blank Br No." (DL38 only) METTLER method "910 Stromboli" (DL38 only) Analysis (<Run> key) Starting a method Menu sequence up to standby mode (KF methods) Standby mode Sample determination Weight transfer from a balance Post consumption Calculations Sample series with statistics (DL38 only) Concentration determination Blank determination Drift determination Bromine number determination (DL38 only) Sample determination with the oven sample changer Stromboli (DL38 only) KF learn titration Auxiliary functions (<Stirrer>, <Burette>, <Pump>, <Results>) <Stirrer> <Burette> <Pump> <Results> All results Recalculation Report Calculations (DL38 only) Statistics (DL38 only) Statistics series (DL38 only) Information menu (<i> key) Error messages, malfunctions and hardware tests Error messages from the titrator Other errors and malfunctions Hardware tests User interface Peripheral interfaces Inputs and outputs METTLER TOLEDO DL31/DL38

5 10 Installation and maintenance Equipping the titration stand Installing the burette Installing the solvent and waste bottles Attaching the magnetic stirrer, electrode and devices Using TTL inputs and outputs (DL38 only) Maintenance and servicing Standard and optional equipment Standard equipment Optional equipment Technical data Index METTLER TOLEDO DL31/DL38 3

6 4 METTLER TOLEDO DL31/DL38

7 The DL31/DL38 KF titrators 1 The DL31/DL38 KF titrators The METTLER TOLEDO DL31/DL38 titrators are microprocessor controlled analytical instruments which you can use to perform Karl Fischer titrations simply, quickly and dependably. You can attach a balance, the METTLER TOLEDO GA42 printer and a computer to the appropriate RS232C interfaces as well as an EPSON- or HP-compatible printer to the Centronics interface and, at the DL38's TTLinterface, the METTLER TOLEDO oven sample changer Stromboli. The METTLER TOLEDO LabX titration software allows you to control your titrator via a computer. The titrators have a tutorial stored which quickly enables you to become acquainted with the operation and method of functioning of the instrument. The two titrators have the same operation. Differences in the hardware and software are mentioned in the corresponding sections. These Operating Instructions correspond to software version 2.0 or higher. Where can you find what information? These Operating Instructions and the Help texts integrated in the titrator provide a complete description of the method of functioning of the two titrators. Explanations of parameters contained in the Help texts are supplemented here when necessary. On the Memo card you can find a short overview of menus and methods. The Application brochure explains the theoretical fundamentals of the Karl Fischer titration, the control of the titration in the DL31/DL38 and documents the METTLER methods stored in the DL38. The Help texts in the titrator provide you with more information or refer you to the Operating Instructions or the Application brochure. You will find a detailed description of the communication between the titrator and a computer in the Description of the computer interface. METTLER TOLEDO DL31/DL38 5

8 Safety measures 2 Safety measures The titrators have been tested for the experiments and intended purposes documented in these Operating Instructions. However, this does not absolve you from the responsibility of performing your own tests of the products supplied by us regarding their suitability for the methods and purposes you intend to use them for. You should therefore observe the following safety measures. 2.1 Measures for your protection Ensure that you plug the power cable supplied into a receptacle outlet that is grounded! In the absence of grounding, a technical fault could be lethal. Risk of electric shock Never work in an environment subject to explosion hazards! The housing of the instrument is not gas tight (explosion hazard due to spark formation, corrosion caused by the ingress of gases). Risk of explosion When using chemicals and solvents, comply with the instructions of the producer and the general lab safety rules! All Karl Fischer reagents are readily flammable and toxic. In the case of skin contact, immediately wash off with copious amounts of water! If eye contact occurs, rinse intensively with copious amounts of water and consult a physician! 2.2 Measures for operational safety Caution Have the instrument serviced only by METTLER TOLEDO Service! Make sure that every connector is in the correct position! Do not damage the connector pins of the magnetic stirrer cable! Pins damaged by faulty insertion can cause a short circuit at the "Stirrer" output. This renders the titrator non-functional. Always wipe off splashed liquids immediately! The instrument is not water-proof. Exclude the following environmental influences: powerful vibrations, direct sunlight, atmospheric humidity greater than 80%, temperatures below 5 C and above 40 C, powerful electric or magnetic fields! 6 METTLER TOLEDO DL31/DL38

9 The titrator 3 The titrator Titration stand Burette Titrant bottle Arrestment knob Pump knob Solvent bottle Waste bottle Keypad Magnetic stirrer Rear view Balance (RS232C) External stand (DV705) GA42 printer (RS232C) Stirrer output Electrode input (KF) Pump unit Suction fitting Computer (RS232C) Stromboli, TBox, etc. (TTL I/O) EPSON- and HP-compatible printers (Centronics) On/Off switch Output fitting Socket for external power pack METTLER TOLEDO DL31/DL38 7

10 The titrator 3.1 Putting into operation Plug the supplied external power pack into the titrator s socket, connect to the power supply and switch on the titrator: A self-test is performed before the name of the titrator appears (example DL38). <Reset> key Reset Display Arrow keys <i> key Auxiliary function keys i Stirrer Pump Burette * Results METTLER TOLEDO DL38 Version 2.0 Hello! Esc F1 F2 F Shift ( ) 8 9 [ ] * CE. Del Entry keys Setup Method Run Menu keys Command keys The command key <F3>, "Hello", the <i> key and all Menu and Auxiliary function keys can be activated after the titrator has been switched on. 3.2 The operating concept Press, e.g. the <Setup> key: Title line Selection bar Resources KF titrants Br No. titrants KF standards Print SETUP OK DL31: No "Br No. titrants"! Name of the key, in other words the displayed list of resources belongs to the Setup menu Commands You can now also activate the arrow key ( ), the <Reset> key and the Command keys <F2>, "Print" and <F3>, "OK". Print OK The arrow in the display means that the list contains more resources. If you press the arrow key ( ), the lines are scrolled upward, the selection bar is fixed. The commands you can execute always refer to the line that is selected. Press <F2>: The list of KF titrants is printed out (if a printer is selected and defined). Press <F3>: The list of KF titrants appears. 8 METTLER TOLEDO DL31/DL38

11 The titrator The command keys The commands which can be triggered with <F1>...<F3> change according to the selected menu item. The following commands require an explanation: Hello! When the instrument is delivered, the <F3> command in the initial mask "METTLER TOLEDO..." is assigned to a Tutorial menu. This is deleted when you have performed the first titration with the Tutorial. Note You can call up the Tutorial at any time with the <i> key. OK This command is always a confirmation for what you wish to view, have viewed or entered, wish to adopt from a selection. Modify When this command appears a submenu can appear which can or must be modified, a selection menu appears from which you can or must accept values or names, an existing parameter value or name can be directly replaced. If a value can be modified or entered only with the keypad, the "Modify" command is missing. ABC This command always appears when you can select letters or characters, e.g. for a name. In this case, you can not enter numbers until you have confirmed "ABC" (press <F1>). Help Information about the selected resource appears. The <Esc> key If you have made changes in the current menu or submenu, they are discarded, in other words Esc the original values/names remain in force. <Esc> always effects a return to the previous display. The <Reset> key The initial mask "METTLER TOLEDO..." reappears: <Reset> is used to terminate analyses or other actions. Data that are not stored are lost. Reset METTLER TOLEDO DL31/DL38 9

12 The titrator The menu keys In order to analyze a sample automatically, the required data must be stored. In the titrator, these data are assigned to so-called task areas, the menus and can be accessed with the Menu keys. It is only the coordination between these menus that makes the automatic analysis possible. Setup All resources required for the titration such as KF titrants and KF standards are stored in the Setup menu and can be changed. Method The sample is determined with the aid of a method. All methods necessary for the different analyses are stored in the Method menu and can be changed. All resources defined in the Setup menu are available for these methods. DL31: Only one method can be stored. DL38: Fifty user methods can be stored. Run The titration is performed in the Analysis menu. The method called up determines the analysis sequence. Note Each menu is subdivided into task areas (submenus) which are designated menus, lists or masks in these Operating Instructions The auxiliary function keys To rinse the burette or recalculate results, the required commands are also assigned to menus. As they are independent of a sample analysis, but can support it, we call them auxiliary functions. They are accessible under the corresponding keys. Stirrer You can switch the stirrer on or off and change the stirring speed. Pump You can add or siphon off solvent. Burette You can rinse the burette and the tip of the dispensing tubing and add a specified volume. * Results You can view the result list of analyzed samples, perform recalculations, change the statistical evaluation of a series (DL38 only!) and print out additional reports. 10 METTLER TOLEDO DL31/DL38

13 The titrator The <i> key The value of the current solvent capacity, the last drift determination, the last blank value i determination for DL38/Stromboli (METTLER method 910), the "Hello!" Tutorial, the KF learn method and a menu for testing the titrator hardware are accessible with this key The entry and arrow keys Shift With the <Shift> key, you can activate the characters above the numbers. CE Del CE Del You delete all entered numbers/characters/letters. You delete the number/character/letter last entered. Shift Shift You can move the cursor to the right or left (only if letters/characters are selected), see example: User a Cursor abcdefghijklm nopqrstuvwxyz ABCDEFGHIJKLM Help Select OK Shift Shift + + skips 3 lines of the display upward (page up), skips 3 lines of the display downward (page down). The arrow appears in the display when there are more lines to the list than are visible. When you press the arrow keys ( ) next to the display, the lines are scrolled downwards or upwards. The selection bar is fixed. By pressing <Shift>, or <Shift>, the lines are moved a page at a time. The commands that can be executed always refer to the line highlighted by the selection bar. METTLER TOLEDO DL31/DL38 11

14 The titrator 3.3 Changing the language All texts in the titrator are stored in English, German, French, Spanish, Italian and Russian. If you have not run the Tutorial and understand one of the available languages better than the one displayed, you should select it: Setup Press the <Setup> key. Resources SETUP KF titrants Br No. titrants KF standards Print OK Resources Peripherals Settings SETUP Press the <Shift> and Arrow ( ) once, then press only the Arrow key to select "Settings". Settings OK SETUP Press <F3>, "OK". Language English User list Date Modify OK Press <F2> repeatedly until, e.g. "Español" appears. Settings SETUP Lengua Español Lista usarios Fecha Modif. OK With "OK" or <Esc> the "Resources" mask reappears. OK Spanish texts appear. Esc English texts appear. 12 METTLER TOLEDO DL31/DL38

15 Setup (<Setup> key) 4 Setup (<Setup> key) In order to perform titrations, the titrator must know the titrants and their concentration. It must know the settings of the attached instruments to transfer the data. In this menu you define and store these resources: You set up your titrator. When you press the <Setup> key, the list of resources appears: KF titrants Br No. titrants (DL38 only) KF standards Main methods (DL38 only) Peripherals Settings The most commonly used titrants and KF standards are already stored in the titrator. You can not only delete these or change their parameters, but also define new ones. All titrants and KF standards needed for the METTLER methods are stored! If you delete one of these resources, the error message that it is missing does not appear until the start of the titration. Print OK Depending on your choice of resource, its list with the corresponding parameters will be printed out. The list of the selected resources appears. 4.1 KF titrants With <F3>, "OK" the stored KF titrants appear. 1-comp 5 1 component reagent: 5 mg/ml 1-comp 2 1 component reagent: 2 mg/ml 2-comp 5 2 component reagent: 5 mg/ml 2-comp 2 2 component reagent: 2 mg/ml Pyridine 5 Pyridine (1 component reagent): 5 mg/ml 1-comp 5K 1 comp. reagent for ketones: 5 mg/ml... free line for a new titrant METTLER TOLEDO DL31/DL38 13

16 Setup (<Setup> key) Delete Print Modify Name Conc. Type Burette Batch The titrant is deleted. The parameters of the titrant are printed out. The parameters of the titrant appear: Name 1-comp 5 Conc.[mg/mL] Type 1 component Burette 5 ml Fill rate [%] 100 Batch Check after [day] 0 Date Time 0:00 Press <F1>, "ABC" to change the name. The titrant with its parameters will be stored under this name. You can change the concentration or its range. You should change the concentration only if you know the correct value! Select one of the preset titrant types: 1 component, 2 components, Pyridine and Others. The correct selection is important (see "Control parameters", Section 5.2). Select the burette (volume) which is used to dispense the titrant. Press <F1>, "ABC" to enter the batch number specified on the bottle. Storage procedure The titrant with its changed parameters is stored when you confirm the parameter list with <F3>, "OK". If you press the <Esc> key, no changes will be made. New KF titrant You add a titrant to the titrant list when you confirm the free line with <F3>, "OK" The parameters always appear, only the name of the titrant is missing. Change the parameters as described above. The name of the new titrant must differ from those already stored, otherwise an existing titrant will be overwritten! Note In the DL31 you can store 10 titrants, in the DL METTLER TOLEDO DL31/DL38

17 Setup (<Setup> key) 4.2 Br No. titrants (DL38 only) With <F3>, "OK" the stored titrants for determination of the bromine number appear: Br - - /BrO 3 Bromide/bromate solution... free line for a new titrant Delete Print Modify Name Burette Batch The titrant is deleted. The parameters of the titrant are printed out. The parameters of the titrant appear: Name Br - - /BrO 3 Conc. [mol/l] 0.05 Burette 5 ml Fill rate [%] 100 Batch Press <F1>, "ABC" to change the name. The titrant and its parameters will be stored under this name. Select the burette (volume) which is used to dispense the titrant. Press <F1>, "ABC" to enter the batch number specified on the bottle. Storage procedure The titrant with its changed parameters is stored when you confirm the parameter list with <F3>, "OK". If you press the <Esc> key, no changes will be made. New Br No. titrant You add a new titrant to the titrant list when you confirm the free line with <F3>, "OK". The parameters always appear, only the name of the titrant is missing. Change the parameters as described above. The name of the new titrant must differ from the one already stored, otherwise an existing titrant will be overwritten! Note You can store 5 titrants for the bromine number. METTLER TOLEDO DL31/DL38 15

18 Setup (<Setup> key) 4.3 KF standards With <F3>, "OK" the stored Karl Fischer standards appear which you can use to determine the concentration of the KF titrants. di-na tartrate di-sodium tartrate. 2 H 2 O H 2 O standard 10 Water standard : 10 mg/g H 2 O standard 1 Water standard: 1 mg/g H 2 O standard 5 Water standard: 5 mg/ml H 2 O ISO 3696 pure water following ISO standard... free line for a new standard Delete Print Modify Name Batch Type Weight The standard is deleted. The parameters of the standard are printed out. The parameters of the standard appear: Name di-na tartrate H 2 O content Unit % Batch Type Mass Weight [g] Press <F1>, "ABC" to change the name. The standard and its parameters will be stored under this name. Press <F1>, "ABC" to enter the batch number specified on the bottle. You can select mass or volume. "Weight" changes accordingly to "Volume". Optimum values for a titrant concentration of 5 mg/ml and a burette volume of 5 ml are stored: 0.05 g for the tartrate standard, 0.75 g for the H 2 O standard 10, 3.5 g for the H 2 O standard 1, 0.01 g for the H 2 O standard ISO 3696, Volume 3 ml for the H 2 O standard 5. Storage procedure The standard with its changed parameters is stored when you confirm the parameter list with <F3>, "OK". If you press the <Esc> key, no changes are made. New KF standard You can add a standard to the list of KF standards if you confirm the free line with <F3>, "OK". The parameters always appear, only the name of the standard is missing. Change the parameters as described above. The name of the new standard must differ from those already stored, otherwise an existing standard will be overwritten! 16 METTLER TOLEDO DL31/DL38

19 Setup (<Setup> key) Note In the DL31 you can store 10 standards, in the DL The Application brochure offers tips on sample preparation, sampling and the optimum amount of sample. 4.4 Main methods (DL38 only) When the titrator is delivered, the <F3> command is assigned to the Tutorial "Hello!", in other words you can select its sequence immediately. In this menu you can assign methods to command keys <F1>...<F3> or delete "Hello!". With <F3>, "OK", the following appears (example on delivery of the titrator): Main methods SETUP F1: Free Modify OK With <F2>, "Modify", the following appears: Main methods SETUP User methods METTLER methods OK Main methods SETUP F1: Method 910 Title Stromboli You can select a method from the METTLER methods (or from the user methods if available), e.g. "910 Stromboli": Delete Modify OK With <F3>, "OK", the following appears: Main methods SETUP F2: Free Modify OK You can select a different method to configure the <F2> command (press <F2>, "Modify"). If you confirm this display with <F3>, "OK", the following appears: Main methods SETUP F3: Hello! Delete Modify OK You can either delete "Hello!" with <F1> or overwrite it by a different method (press <F2>, "Modify"). METTLER TOLEDO DL31/DL38 17

20 Setup (<Setup> key) 4.5 Peripherals With <F3>, "OK" the names of the instruments which you can attach to the titrator via the RS232C interfaces, the Centronics interface, the stirrer output and the DV705 connection appear. You must define these and possibly change the preset settings. Printer Balance Titrn stand Computer If you have the METTLER TOLEDO oven sample changer Stromboli connected to the TTL I/O interface, no further entries are necessary Printer With <F3>, "OK" the names of the printers which you can attach to the titrator appear. HP GA42 EPSON None Select the attached printer. With an EPSON or HP printer change the type and possibly the settings with <F2>. Type Select "PCL3+", "PCL3", "LQ/Stylus" or "LX/SX" Paper Select "Single sheet" or "Fanfold" (see "Feed") Format A4 width = 21 cm, length = 29.7 cm 8 1 / 2 * 11" width = 8 1 / 2 inches, length = 11 inches 8 1 / 2 * 12" width = 8 1 / 2 inches, length = 12 inches Feed Select "Yes" or "No". Yes Each report starts on a new page; with "Paper: Single sheet" a footer is printed out on each page. No The individual reports are separated by a distance of 2 lines. If you select an EPSON- or HP-compatible printer, you must enter the following settings: Standard settings for the printer are printed in bold HP-compatible EPSON-compatible Type PCL3+ or PCL3 LQ/Stylus or LX/SX Paper Single sheet Single sheet or Fanfold Format A4 or 8 1 / 2 * 11" A4, 8 1 / 2 * 11" or 8 1 / 2 * 12" Automatic feed Yes Yes or No 18 METTLER TOLEDO DL31/DL38

21 Setup (<Setup> key) Balance Unidirectional Bidirectional None Unidirect. On request for the weight, the balance continuously transfers the current weight value. Titrator Data to titrator Balance Configuration: "Send Cont." Bidirect. On request for the weight, the balance transfers the current weight value when ordered by the titrator. Titrator Command from titrator Data to titrator Balance Configuration: "Send Stable" ("Send on Transfer") With METTLER TOLEDO balances AB, AG, AT and AX always use the setting "Bidirectional" and the following settings on the balance: Baud rate: 2400, Data bits: 7, Parity: Even, Handshake: No Titration stand Internal External As an external titration stand you can attach the DV705 KF Titration Stand from METTLER TOLEDO whose magnetic stirrer and pump are controlled via the DV705 connection ("External stand") Computer Defined Not defined If you attach a computer, you must select "Defined" and possibly change the settings. Baud rate Select 1200, 2400, 4800 or Parity Select "Even", "Odd" or "None". Data bits Select 7 or 8 bits. Stop bits Select 1 or 2 bit(s). Character set Select "ASCII" or "DL". Note If you select "DL", you must specify 8 for the number of data bits! Start/end Select "'{'/CR" or "STX/ETX". METTLER TOLEDO DL31/DL38 19

22 Setup (<Setup> key) Default settings for the computer Baud rate 4800 Parity Even Number data bits 8 Number stop bits 1 Character set ASCII Start/end '{'/CR Note The METTLER TOLEDO LabX titration software allows you to control your titrator via a computer. You will find additional information on the communication between titrator and computer in the Description of the computer interface. 4.6 Settings You can or must select or define the following settings for the titrator: Language User list Date Time Titrator ID Access for Beep Solv. capac.[ml] Pumping time [s] Language Select English, German, French, Spanish, Italian or Russian. User list Date Time Press <F2>, "Modify", and a list of defined names and an empty line (" ") appears where you can enter a new name. Press "ABC" and you can enter your name. Erase a selected name with "Delete". You can then select your name for both the development of a method and the performance of the analysis. You can set the date and select the format. Day 26 Month 8 Year 1998 Format Format Select " ", "08/31/1998", "31-Aug-1998" or "Aug/31/1998". You can set the time and select the format. Hour 10 Minute 20 Format 24 h Format Select "24 h" or "am/pm". 20 METTLER TOLEDO DL31/DL38

23 Setup (<Setup> key) Titrator ID Access for Beep Solv. capac. Pumping time To enter an identification for your titrator, press <F1>, "ABC". The ID is always reported. You can decide whether all persons who work with the titrator should also have access to the Setup and Method menus, in other words have the right to modify resources or methods. Expert When the titrator is delivered, you have access to all menus. To change this, select "Routine". Routine You can in the Setup menu only print out the defined resources and view the list of settings. in the Method menu only print out the list of methods (DL38 only) and each method. in the Results menu not perform any recalculation and not change any statistical data. under the <i> key, select neither the Tutorial, the KF learn titration nor the Hardware tests menu. Renewed access for experts is described on the last page of these Operating Instructions. You can select: Yes Minimum No Minimum Yes A beep sounds on transition from pretitration to standby, on display of the results and in the case of error messages. A beep also sounds after each keystroke. You can perform several titrations in the same solvent in succession, but its capacity is limited. In the vicinity of the capacity limit, the reaction rate decreases. You should enter a value for the maximum titrant volume which is suitable for your sample determinations. If this value is exceeded, the error message "Solvent capacity exhausted" appears. Only the titrant volume which is consumed during the analysis is summed. The volume which is added, e.g. using the auxiliary function "Dispense" is not taken into account. The difference between the defined value and the titrant consumption is shown under the <i> key. The defined time is a safety criterion: the pump will shut off after this time if you, e.g. leave the titrator while the pump is running. METTLER TOLEDO DL31/DL38 21

24 Methods (<Method> key) 5 Methods (<Method> key) The titrator automatically performs analyses with the help of predefined methods. On delivery of the instrument in the DL31 the KF standard method specified by us is stored. You can modify this method and save it under a number. in the DL38 the KF standard method specified by us and 11 METTLER methods are stored. You can modify these methods and save them as user methods. Methods METHOD Methods METHOD KF standard method Help Method METHOD No. 0 of the method Help OK When you have modified and saved the method, the following appears (example): Methods Modify METHOD User methods METTLER methods KF standard method Help Print OK Print The list of methods you have developed is printed out. OK The user methods with their defined numbers and titles appear (example): Methods METHOD 22 Coffee 33 Tea 113 Powdered milk Delete Print Modify 123 Cellulose KF standard method Print Modify A complete titration method comprises sample preparation, mixing and wait times, the actual titration, result calculation and a report. These partial steps are defined in the titrator as parameters which determine the progress of an analysis. You modify a method by changing its parameters. 22 METTLER TOLEDO DL31/DL38

25 Methods (<Method> key) 5.1 The KF standard method You can use the KF standard method to develop your own method. In this you are guided from one parameter to another in the specified order. Exceptions are sample, control, termination and report parameters, which are shown as a group in a mask. In the case of the DL38, this also applies to the calculation parameters. With the user and METTLER methods, all parameters appear as a list in a mask. Exceptions are again the above-mentioned groups. The last parameter of a method "Author of the method" always appears in its own mask. The method is always shown with the following default parameters. The parameters which you can modify are listed in Section 5.2. No. of the method 0 Title of the method Sample parameters ID Type Mass Minimum [g] Maximum [g] Entry Before Speed [%] 35 Mix time [s] 10 Titrant 2-comp 5 Volume [ml] for predisp (Wait time [s] after predisp. 0) Auto start No DL38 only Control parameters Current [µa] 20 End point[mv] 100 Vmin [µl] 0.5 Vmax [µl] 8.0 Vmax factor [%] 30 Start Cautious Termination param. Max. time [s] 600 Drift stop Rel. Drift [µg/min] 15 Vmax [ml] Blank [µg] 0 Drift Online Result % DL31 only Calculation 1 % R1 = x [%]*f1 f1 = Unit % Decimal places 2 Statistics Yes Max. srel [%] 0.00 Calculation 2 R2 = No calculation f2 = Unit DL38 only Decimal places 2 Statistics Yes Max. srel [%] 0.00 Calculation 3 R3 = No calculation f3 = Unit Decimal places 2 Statistics Yes Max. srel [%] 0.00 Standby Yes Report Output Print.+Comp. Type GLP Author of the method The METTLER methods and specific parameters for automation with the METTLER TOLEDO oven sample changer Stromboli are described in a separate chapter. METTLER TOLEDO DL31/DL38 23

26 Methods (<Method> key) 5.2 KF method parameters The following parameters can be changed. This will either cause some parameters to appear or disappear No. (of the method) The method is stored under this number. The numbers are reserved for METTLER methods Title (of the method) You can give the method a specific name Sample parameters ID You can enter an identification for the sample(s) now or just before the titration for every sample ("Request"). Type Select "Mass", "Fixed mass", "Volume", "Fixed volume", "Pieces" or "Fixed pieces". Weight appears when "Fixed mass" is selected. Volume appears when "Fixed volume" is selected. Number appears when "Fixed pieces" is selected. Density appears when "Volume" or "Fixed volume" is selected. Minimum/Maximum appears when "Mass", "Volume" or "Pieces" is selected. The unit depends on the type of sample: Entry g, ml or pcs. <F1>, "Help" For a fixed or variable amount of sample you can have the titrator calculate and enter values if you know the approximate water content of your sample. of the amount of sample before or during the actual titration. "Entry" is faded out when "Fixed mass", "Fixed volume" or "Fixed pieces" is selected. DL38: If you select "Yes" for the parameter "Auto start", on storage "Before" is automatically set to "During" Speed Stirring should guarantee quick and thorough mixing of the electrolyte. We rocommend the setting: 40%. The magnetic stirring rod should not "jump". Only use the magnetic stirring rod included in the delivery Mix time This value for time is an empirical value and can be entered specific to the samples ("Request") Titrant You can select from the titrants stored in the Setup menu. 24 METTLER TOLEDO DL31/DL38

27 Methods (<Method> key) Volume (for predispensing) A predispensing shortens the titration time and can be entered specific to the sample ("Request"). Note In the user and METTLER methods the parameter is called "Predis." Wait time (after predispensing) The parameter does not appear in the KF standard method if you have entered "0" for the predispensing. This parameter always appears in the user methods Auto start (DL38 only) Yes The DL38 begins analysis as soon as a sample has been added. The time for adding a sample may not exceed 30 seconds or the instrument will revert to its "Standby" mode. You should select "Yes" for determinations in which, e.g. side-reactions could occur during the titration Control parameters The following holds for all control parameters: You should not modify the preset default values for the different reagent types until you have evaluated the titration curve of your sample (see Application brochure). 1 component 2 components Pyridine Current 20 µa 20 µa 20 µa End point 100 mv 100 mv 100 mv Vmin 0.5 µl 0.5 µl 0.5 µl Vmax 4.0 µl 8.0 µl 3.0 µl Vmax factor 100% 30% 100% Note Vmin and Vmax depend on the burette volume; the values listed apply to the 5 ml burette. In the Tutorial and KF standard method these default values are automatically entered for the selected titrant and hence the type. This does not apply to user methods: When you select a titrant whose type differs from the previous one, you should also adapt the control parameters. Current Select 1, 2, 5, 10, 15, 20, 30 or 40 µa for polarization current Termination parameters To terminate the titration you must define "Vmax" and "Drift stop" ("Delay" respectively) as a condition; the maximum time is an additional termination condition. The titration is terminated when the first of the selected conditions is met. METTLER TOLEDO DL31/DL38 25

28 Methods (<Method> key) Vmax Drift stop Delay The maximum volume is intended as a safety precaution: It avoids dispensing an unnecessarily large amount of titrant if the titration is faulty. Select "Relative", "Absolute" or "No". Relative Termination when actual drift is less than the drift measured before the titration (D 0 ) plus the entered value (D i ): D < D 0 + D i. Absolute Termination when the drift is less than the entered value (D i ): D < D i. No "Drift [µg/min]" disappears and "Delay [s]" appears. If you enter "0" for the delay time, the titration is terminated as soon as the end point is reached Blank For the entry of a correct value, you should perform a determination. [µg] You can enter a value in the method. Request Before each titration, the value is requested individually for each sample Drift The drift value is needed for calculation of the result. [µg/min] You can enter a value in the method. Request Before each titration, the value is requested individually for each sample. Online The moisture which enters the titration vessel is always measured, evaluated and displayed in the standby mode. Determin. Some standard operating procedures require insertion of the value of a drift determination. If you have performed a drift determination, the result is stored under the <i> key and used in the calculation Result (DL31 only) The water content is calculated with the appropriate formula by selection of the unit: [mg], [µg], [%], [ppm], [mg/pc], [mg or µg] and [% or ppm]. [mg or µg], [% or ppm] With the following limit values, the result is automatically set from one unit to the other: mg µg % ppm less than less than greater than greater than Calculation (DL38 only) Calculation 1 R1 Result of the first calculation. The water content is calculated with the appropriate formula by selection of the unit: [mg], [µg], [%], [ppm], [mg/pc], [g/kg], [ml], [min], [ppm]ext.extr., [ppm]ext.soln., [%]ext.extr., [%]ext.soln.. 26 METTLER TOLEDO DL31/DL38

29 Methods (<Method> key) Unit Statistics Max. srel [ml] Titrant consumption up to the end point. [min] Duration of the titration. [ppm]ext.extr., [ppm]ext.soln., [%]ext.extr., [%]ext.soln. Special calculation for samples which are used after an external extraction or external dissolution. The second and third calculation are needed (see Application brochure). You can enter a nonselectable unit, e.g. "g" if you define a factor of for the calculation of the H 2 O content in "mg". To obtain the mean value "x", the standard deviation "s" and the relative standard deviation "srel" of a sample series, you must select "Yes". You can terminate a sample series using the auxiliary function "Results" (<Results> key). If the entered value for the max. relative standard deviation is exceeded, a message appears. Calculation 2 / Calculation 3 The available parameters are the same as for Calculation 1. Instead of a formula, you can select "No calculation". The following units are missing: [ppm]ext.extr, [%]ext.extr., [ppm]ext.soln, [%]ext.soln. Note You can not determine samples from an external extraction or dissolution in the routine mode as you must enter the amount of sample for the extraction/dissolution and the amount of solvent under calculation 2 and Standby Yes No [min] After a titration, the titration vessel is kept anhydrous. We recommend allowing the standby titration to run even during lengthy pauses so that you can start the next titration at any time. After a titration the start mask of the Analysis menu reappears. After the sample determination, a switch is made to the "Standby" mode. The subsequent rate of consumption is displayed and printed out during the defined time Report Output Select "Printer", "Computer" or "Print.+Comp." as output device. Type DL31: Select "GLP", "Short-form" or "None". DL38: Select "GLP", "GLP+curves", "Short-form" or "None". Curves can be printed out only on an EPSON or HP-compatible printer. (GLP report: All data which are required by the rules of Good Laboratory Practice.) Author of the method The selection of your name documents that you are responsible for the development of the method. METTLER TOLEDO DL31/DL38 27

30 Methods (<Method> key) 5.3 Storage procedures The following always appears as the last parameter of a method: Method METHOD Author of the method Help Modify OK The modified method is stored when you confirm by pressing <F3>, "OK". Examples: DL31 DL38 Methods METHOD Methods METHOD 123 CaCl 2 KF standard method Help Print Modify 4 H 3 PO 4 31 Oil Delete Print Modify If you have not entered any or a wrong method no., the following appears: Error No/invalid value Min: Max: OK Confirm the error message by pressing <F3>, "OK". Method METHOD No. 0 of the Method Help OK Enter the new number and confirm by pressing <F3>, "OK". The method is stored. 28 METTLER TOLEDO DL31/DL38

31 Methods (<Method> key) If you have entered a method No. which already exists, the following appears: DL38 Method 22 METHOD Method No. exists Change number Overwrite method OK Change number Overwrite method "No. of the method" reappears. The new or modified method is stored, that with the same number deleted. While you are modifying a user or a METTLER method, you can press the <Run> key (the <Setup> and Auxiliary functions keys are blocked). a. If you have not yet modified any parameter of the method, the start mask of the Analysis menu appears. b. If you have already modified a parameter of the method, the mask "Author of the method" appears. The method is stored with "OK" and the start mask of the Analysis menu is displayed. METTLER TOLEDO DL31/DL38 29

32 Methods (<Method> key) 5.4 User and METTLER methods (DL38 only) The following methods have been developed by METTLER TOLEDO and can be performed immediately (see Application brochure). 900 Standard Na tartrate 902 Toluene dry 903 Ketone 904 Homogenizer 905 Ext. Extr. 906 KF Oven 907 Gas 908 Bromine No. 909 Blank Br No. 910 Stromboli You can modify METTLER methods, but in this case you must always give them a number (1-899) so that they are stored as user methods. You can print out the selected methods by pressing <F2>, "Print". User methods can be deleted (only in expert mode). Methods METHOD 22 Coffee 33 Tea 113 Powdered milk Delete Print Modify If you press <F1>, "Delete", the following appears: Delete? METHOD Yes No OK Yes No Pressing <F3>, "OK", will delete the method. Pressing <F3>, "OK", will bring up the list of methods. The method is not deleted. METTLER methods cannot be deleted. Methods METHOD 900 Standard Na tartrate 902 Toluene dry Print Modify 30 METTLER TOLEDO DL31/DL38

33 Methods (<Method> key) METTLER methods "908 Bromine No." and "909 Blank Br No." (DL38 only) If you wish to develop a bromine number determination to meet your requirements, you can modify METTLER method 908 or 909 and store as user methods. The "909 Blank Br No." method's result serves as blank value for the bromine determination. No. 908 Title Bromine No. Sample parameters ID Request Type Mass Minimum [g] Maximum [g] Entry Before Speed [%] 30 Mix time [s] 120 Titrant Br-/BrO 3 - Predisp. [ml] Wait time [s] 0 Control parameters Current [µa] 2 End point [mv] 150 Vmin [µl] 1.0 Vmax [µl] 20.0 Vmax factor [%] 100 Start Normal Termination param. Max. time [s] 6000 Delay [s] 15 Vmax [ml] Blank Request Calculation 1 R1 = x[br No.]*f1 f1 = Unit Decimal places 2 Statistics Yes Max. srel [%] 0.00 Calculation 2 ml R2 = x [ml]*f2 f2 = Unit ml Decimal places 3 Statistics No Max. srel [%] 0.00 Calculation 3 R3 = No calculation f3 = Unit Decimal places 2 Statistics Yes Max. srel [%] 0.00 Report Output Print.+Comp. Type GLP Author of the method Type Select "Mass", "Fixed mass", "Volume" or "Fixed volume". Weight appears when "Fixed mass" is selected. Volume appears when "Fixed volume" is selected. Density appears when "Volume" of "Fixed volume" is selected. Min./Max. appear when "Mass" or "Volume" is selected. The unit depends on the type of sample: [g] or [ml]. Entry of the amount of sample before or during the actual titration. "Entry" is faded out when "Fixed mass" or "Fixed volume" is selected. No. 909 Title Blank Br No. Sample parameters ID Request Type Fixed volume Density [g/ml] Volume [ml] 50 Speed [%] 30 Mix time [s] 120 Titrant Br - - /BrO 3 Predisp. [ml] Wait time [s] 0 Control parameters Current [µa] 2 End point [mv] 150 Vmin [µl] 1.0 Vmax [µl] 5.0 Vmax factor [%] 100 Start Cautious Termination param. Max. time [s] 6000 Delay [s] 15 Vmax [ml] Calculation 1 mmol R1 = x [ml]*f1 f1 = Unit mmol Decimal places 4 Statistics Yes Max. srel [%] 0.00 Calculation 2 R2 = No calculation f2 = Unit Decimal places 2 Statistics Yes Max. srel [%] 0.00 Calculation 3 Report Output Print.+Comp. Type GLP Author of the method METTLER TOLEDO DL31/DL38 31

34 Methods (<Method> key) R1 Unit Author Result of the first calculation. The bromine number or bromine index is calculated using the appropriate formula by selection of [Br No.] or [Br index]. [ml] Titrant consumption up to the end point. [min] Duration of the titration. Bromine number and bromine index are quantities without dimension. The bromine number is the amount of bromine in [g] reacting with 100 g of sample. The bromine index is the amount of bromine in [mg] reacting with 100 g of sample. "Author of the method" only appears if you change the method METTLER method "910 Stromboli" (DL38 only) If, according to your needs, you wish to develop an automated determination of water content of thermally stable liquids or solids, then you can modify the METTLER method "910 Stromboli" and store it as a user method. No. 910 Title Stromboli Sample parameters Type Mass Minimum [g] Maximum [g] Speed [%] 40 Mix time [s] 300 Set temperature 150 Titrant 1-comp 5 Control parameters Current [µa] 5 End point [mv] 100 Vmin [µl] 0.5 Vmax [µl] 4.0 Vmax factor [%] 100 Start Cautious Termination param. Max. time [s] 600 Driftstop Rel. Drift [µg/min] 10 Vmax [ml] Blank Auto Drift Auto Calculation 1 ppm R1 = x [ppm]*f1 f1 = Unit ppm Decimal places 3 Statistics Yes Max. srel [%] 0.00 Calculation 2 Calculation 3 Report Output Print.+Comp. Type GLP Author of the method Sample parameter Mix time Auto start Set temperature The sample parameters "ID" and "Enter" are not applicable, because the sequence of the sample series is controlled automatically. The time (in seconds) during which the water in the sample evaporates completely and dissolves into the solvent in the titration vessel. This parameter does not apply because the sequence of the sample series is controlled automatically. Enter in C at the desired temperature at which the water determinations are to be performed. The set temperature can be selected between 50 C to 300 C. This setting cannot be changed during a series. The set temperature is noted in the titration protocol. 32 METTLER TOLEDO DL31/DL38

35 Methods (<Method> key) Blank Drift Standby Protocol Author The blank [µg] is made up of the water content of the purge gas (time-dependent) and the water content of the sample vessel (independent of time). The determination is performed as a "normal" sample determination with the defined method parameters and, therefore, can be integrated into the series sequence. The product of drift and duration (Drift * Duration) is subtracted from the result, so that the blank is an absolute value independent of time. The blank for the Stromboli can be viewed at any time by pressing the <i> key. Request The value is retrieved prior to the series. Auto The value is determined automatically prior to the sample series ("Blank" position on the sample rack). The result is stored under the <i> key and automatically integrated into the calculations. Determination The most recently stored value is used. Note A one-time blank determination can be used for various sample series. In order to do this, a method with the method parameter "Blank: Auto" is developed. In the request for the sample parameters enter "0" for the number of samples. The resulting blank value is stored and can be viewed at any time by pressing the <i> key, i.e., it is available for all ensuing sample series. The drift [µg/min] can be determined at any time in the STANDBY mode (press <F1>, "Drift") or automatically prior to a sample series. Request The value is retrieved prior to the series. Auto Determination The value is determined automatically prior to the sample series ("Drift" position on the sample rack). The result is stored under the <i> key and automatically integrated into the calculations. The most recently stored value is used. This parameter does not apply as no post consumption measurements are performed. The results are printed out at the end of a series. "Author of the method" only appears if you change the method. At the beginning of a sample series, the following parameters need to be entered, provided you chose "Request" in the method: Mix time [s] Blank [µg] Drift [µg/min] ID [Text] No. of samples [max. 13] Sample parameters (mass, volume, amount, etc.) METTLER TOLEDO DL31/DL38 33

36 Analysis (<Run> key) 6 Analysis (<Run> key) You perform titrations with a selected method. The required data are stored in the Method and Setup menu. You prepare your sample, titrate and obtain the result. While an analysis is running, all menus and auxiliary functions are blocked. 6.1 Starting a method Preparations Press the <Burette> key. Rinse the burette and fill ensuring that there are no air bubbles in the burette and tubing. Press the <Pump> key and fill the titration vessel with approx. 40 ml solvent. When you press the <Run> key, the start mask appears: DL31 DL38 Start RUN Start RUN Method No. 22 Title User Help OK Method No. 22 Title User Help Modify OK As method number "0" is entered if no method (DL31) or no user method (DL38) is stored. in the DL31 case always that of the stored method is automatically entered together with the title. in the DL38 case the number which you enter directly or accept it with <F2> from the METTLER or user methods is entered. Note You can select the user name. The name which was selected in the analysis last performed remains stored. If you have defined an expiry date for the titrant and this has been passed, an appropriate message appears before the pretitration starts. You should then first perform a concentration determination. DL38: The start mask always shows the number of the method with which an analysis was last performed, e.g. Method No. 22. If you delete this, "Method not available" appears when you confirm the mask with "OK". 34 METTLER TOLEDO DL31/DL38

37 Analysis (<Run> key) Start Data RUN transfer.. The titrator also accepts methods which are stored in the attached computer: When you enter a number whose method is not stored in the titrator, the method is requested from the computer (see Description of the computer interface). If it is available, the pretitration is started immediately following transfer; if it is not available, "Method not available" appears Menu sequence up to standby mode (KF methods) Example: Start RUN Method No. 22 Title Coffee User C. De Car Help Modify OK PRETITRATION RUN DL31: "Modify", is missing. The pretitration starts with <F3>, "OK": It is always executed with the control parameters of the selected method. The length of the solid bar reflects the addition of the titrant. The vertical bar represents the threshold for the transition to the standby mode. Help STANDBY RUN Active method:22 Potential [mv]74 Drift µg/min] [ 2 DRIFT CONZ Sample This arrow indicates that you can start a determination. Wait, drift still decreasing! Wait, drift increasing again! Press <F1> to start the drift determination, <F2> to start the concentration determination, <F3> to start the sample determination. Note If the pretitration lasts longer that 10 minutes, a message appears. After confirmation with "OK", a pretitration again starts. In such a case, you should check whether, e.g. all connections of the titration stand are tight. METTLER TOLEDO DL31/DL38 35