PC Control / Touch Control Manual 8.840.
CH-9101 Herisau/Switzerland E-Mail info@metrohm.com Internet www.metrohm.com PC Control Touch Control Program version PC Control 5.0 Touch Control 5.840.0140 Manual 8.840.8003EN 05.
Teachware Metrohm AG CH-9101 Herisau teachware@metrohm.com This documentation is protected by copyright. All rights reserved. Although all the information given in this documentation has been checked with great care, errors cannot be entirely excluded. Should you notice any mistakes please send us your comments using the address given above.
Contents Table of contents 1 Introduction .......................................................... 1 1.1 Instrument description...................................................................................2 1.2 About the documentation ..............................................................................3 1.2.1 Symbols and conventions........................................................................3 2 Installation ........................................................... 5 2.
Contents 3.8.6 3.8.7 3.8.8 3.8.9 3.9 Tubing parameters and parameters for the preparation procedure.....45 Rotating direction of the valve disk (Dosing unit only) ..........................48 Monitoring the GLP test .........................................................................49 Monitoring the working life .....................................................................49 Sensors........................................................................................................ 50 3.
Contents 3.14.5 3.14.6 3.14.7 3.14.8 Output lines ......................................................................................... 101 Custom calibration buffers .................................................................. 103 Report header...................................................................................... 104 Custom electrode type........................................................................ 105 3.15 Loading methods .............................................
Contents 3.22.1 3.22.2 Properties of the result silo ..................................................................164 Saving and loading the result silo........................................................166 3.23 Print……..................................................................................................... 167 3.23.1 Sending or saving a PC/LIMS report ...................................................174 3.23.2 Printing PDF reports...................................................
Contents 4.11.1 4.11.2 4.11.3 4.11.4 Scanning lines (SCAN)........................................................................ 278 Setting lines (CTRL)............................................................................. 278 Receive data (SCAN RS)..................................................................... 279 Send data (CONTROL RS).................................................................. 279 4.12 Automation ....................................................................
Contents 6.1.4 6.1.5 6.1.6 6.1.7 Safety specifications ............................................................................305 Electromagnetic compatibility (EMC) ..................................................306 Ambient temperature ...........................................................................306 Dimensions ..........................................................................................306 6.2 Remote box..................................................................
Contents List of illustrations Fig. 1.1: The Titrando system ................................................................................................... 1 Fig. 2.1: Front view of the Touch Control.................................................................................. 6 Fig. 2.2: Rear view of the Touch Control .................................................................................. 7 Fig. 3.1: Different ways of navigation on the Touch Screen......................................
Contents VIII PC Control / Touch Control
1 Introduction 1 Introduction This manual gives you a comprehensive overview of the functions of the Touch Control and the PC Control software for operating the Titrando system. The Titrando system can either be operated with the Touch Control with touch-sensitive screen as a stand-alone-system or with the PC software PC Control. In this case the varied possibilities of a computer can be utilized. Figure 1.1 shows the versatility of the Titrando system.
1.1 Instrument description 1.1 Instrument description There are two different ways of operating the Titrando system: with Touch Control the operation is via a touch-sensitive screen. A computer with installed PC Control software is a version with several additional features which directly utilize the communications and storage facilities of a PC. The import of Titrino methods is only possible with the PC Control software. Both programs have a context-sensitive online help function.
1 Introduction 1.2 About the documentation Attention! Please read through this documentation carefully before putting the instrument into operation. The documentation contains information and warnings which have to be followed by the user in order to ensure safe operation of the instrument. 1.2.1 Symbols and conventions The following symbols and styles are used in this documentation: 9 Numbers of the parts and controls see illustrations in Section 2.2.
1.
2 Installation 2 Installation Connecting the Touch Control to the Titrando is described in the manual for the Titrando as well as the setup of the titration system with peripheral devices such as stirrers and dosing devices. 2.1 2.1.1 Setting up the Touch Control Packaging The Touch Control and its specially packed accessories are supplied in very protective special packaging. Please store this packaging in a safe place; it is the only way in which the safe transport of the instrument can be guaranteed.
2.2 Touch Control parts and controls 2.2 Touch Control parts and controls Fig. 2.1: Front view of the Touch Control 6 1 Protective cover for card slots Accommodates two PCMCIA or CompactFlash memory cards. 6 Fixed key [START] Starts the current method. 2 “ON” LED Lights up when instrument is switched on. 7 Fixed key [STOP] Stops the run. 3 Touch Screen display 8 Fixed key [Manual] Opens the dialog for manual operation of the titration system. 4 Fixed key [Home] Changes to main dialog.
2 Installation Fig. 2.2: Rear view of the Touch Control 1 Protective cover for card slots Must be closed during operation to protect the electronics from splashes. 14 Contrast controller for display 11 On/Off switch Touch Control must be shut down properly by switching it off before the current supply is interrupted. 15 Connection cable for connecting the Touch Control to the Titrando ("Controller" connection). 12 Card slot 2 Accommodates one PCMCIA or CompactFlash memory card.
2.
3 Operation 3 Operation The most important points concerning the operation of the Touch Control and PC Control are described in this section. As the appearance of the operator interface and the functions are almost identical, only the PC Control operator interface is shown. If individual functions are only available in Touch Control or in the PC Control software then this is indicated accordingly in the text.
3.1 Operating principles: Touch Control 3.1.2 Setting the display contrast of the Touch Control Knob 14 for setting the contrast of the Touch screen is located on the rear panel of the instrument. Move it in one direction and hold it tight when it reaches the stop in order to increase or reduce the contrast. Use the fixed key [Help] in the main dialog to open the online help. Set the contrast so that the scroll bar surface is light gray and the margins to the left and below are dark gray (see Section 3.3.
3 Operation 3.1.4 Entering text and numbers using Touch Control Just touch an input field, e. g. User in the main dialog, to open the Text editor. In the text editor the name of the parameter is shown in front of the input field. Touch the required character. Apart from the capital letters which first appear, there are also sets of characters with lower case letters, numbers and mathematical signs as well as three blocks of special characters.
3.1 Operating principles: Touch Control To the left of the block of numbers you can see the input range together with its default value. If not only numbers but also special values (e. g. off) can be entered for a parameter then the corresponding buttons will be shown to the right of the block of numbers. For many method parameters it is also possible to enter a result which has previously been defined in the method sequence as a value. The result variable can be selected under [R1] (see Section 4.5.1).
3 Operation 3.2 3.2.1 Operating principles: PC Control Starting and stopping the PC Control software A double-click on the PC Control icon, which is automatically copied onto the Windows desktop during installation, starts the program. Alternatively you can start the program in the menu Start/Program Files/Metrohm/PC Control or execute the file PcControl.exe under C:\Program Files\Metrohm\PC Control\bin (installation with the default path) with a double-click.
3.3 User interface and controls 3.3 3.3.1 User interface and controls User interface of the Touch Control and PC Control In both cases the user interface consists of the dialog window itself and the fixed keys. Fig. 3.2: Touch Control user interface Fig. 3.3: PC Control user interface The PC Control program has an additional menu bar.
3 Operation 3.3.2 Controls of the Touch Control and PC Control Both the Touch Control and the PC Control software systems have changing controls within the dialog window and fixed keys outside the dialog window which are accessible at all times. The following table lists the functions of all the controls: Fixed keys Touch Control PC Control Fixed key function Opens the context-sensitive online help function (see Section 3.3.3).
3.3 User interface and controls Dialog elements Touch Control PC Control Fixed key function Active buttons are indicated by a frame. Inactive buttons are shown in gray. Tip or click on a checkbox to activate it. Use the scroll bar in order to navigate quickly through lists or longer text displays. To move up and down in the list push the scroll bar up and down with your finger or with the left-hand mouse key pressed down. The selection list can be recognized by the arrow to the right of the text.
3 Operation 3.3.3 Online help This manual is chiefly intended to describe the procedure for configuring the system, carrying out a determination and evaluating and storing the data. For further details about the individual parameters, e. g. input ranges, you should use the context-sensitive online help, which will rapidly provide you with the information you require at any point. In Touch Control you can open the online help with the [Help] fixed key.
3.4 Program structure 3.4 Program structure The program structure is arranged so that the most important functions can be accessed with only a few clicks or touches on the buttons. Functions which are not often used in routine operation, such as changing the system settings or editing individual parameters in a method, can be found in lower dialog levels.
3 Operation 3.5 Login Depending on how your Titrando system is configured, you may have to use the User login function before you can work with the system. User administration is carried out by a user with administrator rights (see Section 3.7.5 to Section 3.7.7). There are two different ways of identifying the user: by the entry of the user name or by using an identification card, on which the user name and the routine dialog settings are stored.
3.5 Login In Touch Control you must always insert your identification card in Card slot 1. In PC Control ask your system administrator to tell you the drive to be used. If a password additionally has to be entered then the corresponding dialog will be opened automatically; otherwise the main dialog will open directly.
3 Operation 3.6 Main dialog and structure of the dialog windows This section provides an overview of the structure of the dialog windows and the various dialog elements. The user interface without the fixed keys [Help], [Print], [Manual], [STOP], [START], [Home] and [Back] is known as the dialog window (or just dialog): • • In the status line (blue bar) the titles of the previous dialog and current dialog are normally shown.
3.6 Main dialog and structure of the dialog windows A run has been started in the "Manual control" dialog window. A fault has occurred during the manual operation of the System. • • In the main dialog you can enter or select the user if you are not working with login (see Section 3.7.5). You can also edit the sample data (see Section 3.19.1). The buttons at the lower margin of the dialog change their function according to the dialog shown. They are usually used to open a new dialog.
3 Operation 3.7 System settings A range of system-specific settings and configurations is described in this section. You should first select the dialog language and set the date and time. You can also configure the dialog for routine use and create a list of users. You can make various settings concerning the measured value display and output of acoustic signals. 3.7.1 Selecting the dialog language Open the dialog System/System settings.
3.7 System settings Open the editor for the time by touching the input field for the time. Enter the actual time in the format hours:minutes:seconds. The entry should be made in the 24-hour format. The colons already exist. Confirm the entry with [OK]. By entering a local time the time information becomes unambiguous. You can enter the local time for both PC Control and Touch Control. It is printed out in the report header together with the date and time.
3 Operation Note! If you have selected Routine dialog and the dialog System settings/Dialog options is disabled for routine dialog then you can change back to expert dialog by entering Metrohm as the user in the main dialog. If you are using login then a user who works with expert dialog must log in. The selection of method commands (list of commands) and the fixed keys ([Print] and [Manual] only) which can be used can only be opened when the system is being operated in expert dialog.
3.7 System settings method], [Control], [Edit parameter] and [Results]). In order for the button to be active the corresponding checkbox must be activated above. Open the dialog in which you wish to disable buttons and deactivate the checkboxes for the buttons that are to be disabled for routine dialog. You can also disable buttons in several subdialogs. These are indented so that you can see which buttons belong to which dialog. 3.7.
3 Operation Note! If you once have worked with login and password protection then it is no longer possible to delete users from the list even if the password protection is switched off again. The list of users can only be printed out in a context-sensitive situation from the dialog System settings/User administration and its subdialogs by using the [Print] fixed key. This means that only users with administrator rights can print out this list.
3.7 System settings status "Saved" can be signed. The status of the method is given under Method options/Properties (see Section 3.16.9). If use only released methods is activated then the corresponding user can only use methods that have been released, i.e. can only start methods that have been signed at level 2. Review methods (signature level 1) must be activated for a user to be entitled to sign a method at level 1. The method then receives the status "Reviewed".
3 Operation In a similar way to that used for methods, it is possible to state whether a user is entitled to sign determinations at level 1, i.e. to Review determinations, and/or is entitled to Release determinations, i.e. to sign them at level 2. If Delete signatures has been activated for a user then the user is entitled to delete signatures. As in the case of methods, this is only possible when a determination has already been signed at level 2.
3.7 System settings Select the disk drive if you want to use diskettes as identification cards. You can also use a card drive with PCMCIA FlashCards or CompactFlash cards, or a USB memory stick. With external drives you must always check how to recognize when a storage process has been completed in the user manual for the drive. This is usually indicated by an LED.
3 Operation Attention! If you select Login via identification card then you must create an identification card for each user. Once you have selected a login option you can then make further settings for logging in: If a password is to be requested as well as the user name then you must activate the Password required checkbox. If this function is switched on then it is no longer possible to delete users from the list of users; they can only be deactivated.
3.7 System settings If you activate Methods then when a modified method is being saved a reason for the modification will be demanded. Results are altered when a determination is recalculated. If you require a reason to be given in such cases then activate the Determinations checkbox. The reasons are only demanded when login and password is used. These reasons are documented in the audit trail (see Section 3.7.8) together with the alteration.
3 Operation Attention! If a user has forgotten his password, a new user name has to be defined. The same user name can only be used again after a new installation and the recreating of the user list. Proceed therefore as follows: PC Control: Carry out a backup (see Section 3.11.6). If you have defined the PC Control installation directory as location for the backup (under File/Preferences/Paths), copy the folder "Backup" to another position. Uninstall the PC Control software.
3.7 System settings 3.7.8 Audit trail In the Audit trail all user actions are recorded together with the user name, date and time. Recording an audit trail is important for using PC programs to meet the requirements of FDA Guideline 21 CFR Part 11 . Under System/System settings/User administration in the dialog Login options/Audit trail activate the checkboxes for the data to be logged in the audit trail. The actions which should be logged can be found in the online help.
3 Operation Fig. 3.6: Audit Trail The first column shows the number of the entry. The second column for information about shows a symbol which classifies the entry: actions which are neither security-relevant nor alter the determination data; for actions such as logging in and out of the system, changes to the login options and alterations to the determination data such as recalculations; for errors which may occur such as entering an incorrect password during login.
3.7 System settings item Export in the File menu and entering the path and file name with the extension .txt. When the audit trail is exported its contents will be deleted. The audit trail window is closed with Close. To print the audit trail click on the symbol in the symbol bar or choose the report "Audit trail" in the dialog Print/More Reports/System reports. Quick filters can be used on the audit trail entries: Click on a cell in the table which meets the filter criterion.
3 Operation 3.7.10 Acoustic signals • • Open the dialog System settings/Acoustic signals. Show a message: each time that a message appears on the screen a short beep will be heard. This informs the user that the message must be confirmed. This function is switched off by deactivating the checkbox. Button contact (Touch Control only): each time that a button is touched on the Touch Screen this will be confirmed by a beep. If you touch an inactive area of the Touch Screen then no beep will be heard.
3.8 Titrants 3.8 Titrants This section describes how you can draw up a list of titrants used in the system. These titrants can be used in intelligent type dosing units or intelligent type exchange units or in so-called non-intelligent exchange and dosing units. Intelligent exchange and dosing units have a built-in data chip on which data about the reagent and the unit can be stored.
3 Operation In the list of titrants the name, cylinder volume and type, i.e. exchange unit (EU) or dosing unit (DU) are given for every titrant. Intelligent exchange or dosing units are indicated by IEU and IDU and shown in green color (magenta if the line has been selected). For intelligent exchange or dosing units that are attached, the dosing device connection is shown additionally and – if several control devices are configured – the name of the control device appears as well.
3.8 Titrants If you are working with the default settings for the dosing connections then you will also be requested to carry out the "Prep" function in order to rinse all the tubing (see Section 3.24.2). Open the dialog System/Titrants. Open the dosing device selection list, in which new exchange or dosing units are recognized, with [New]. Only one dosing device will normally be shown, unless you have attached several new exchange or dosing units. Confirm the selection with [Select].
3 Operation Enter an unambiguous titrant name under Titrant or select a name from the selection list. Enter the Concentration of the titrant and its units. The titrant concentration can be calculated as the variable CONC in the result calculations (see Section 4.5.1). This is done by selecting a titrant in the titration command for the method (see Section 4.1.5). In a following calculation command you can calculate the concentration of this titrant. You can add a Comment to each titrant.
3.8 Titrants mean value of the determinations has been saved as the titer (see Section 4.5.1). You can monitor the time interval after which the titrants titer must be redetermined. Open the dialog Titer options/Validity and activate the checkbox for Monitoring. Enter either the time interval for the validity of the titer or the date for the next titer determination. When either the time interval or the date is edited the other value will be updated automatically.
3 Operation • • Document message: the fact that the monitoring interval had expired when the determination was carried out will be documented in the determination data. The message can be viewed under Results/More determination data/Messages (see Section 3.18.2). Cancel determination: the determination sequence will stopped and the following message shown: Under Titer options/History the date, time and values of the last ten titer determinations are shown in a table.
3.8 Titrants 3.8.5 Exchange unit and dosing unit Under Edit titrant/Exchange unit and Edit titrant/Dosing unit you can enter data concerning the unit used with the reagent. The data which can be entered here varies according to whether or not an intelligent exchange or dosing unit is used. You can enter a Name for the exchange or dosing unit. The Order number and Serial number are read out automatically in case of intelligent exchange or dosing units.
3 Operation 3.8.6 Tubing parameters and parameters for the preparation procedure Under Exchange unit/Tubing parameters or Dosing unit/Tubing parameters you can enter the lengths and diameters of the connected tubing. With the dosing unit you can also alter the port occupancy.
3.8 Titrants Fig. 3.8: Exchange unit tubing connections Under Exchange unit/PREP parameters and Dosing unit/PREP parameters you can enter the parameters for carrying out the preparation (PREP command) and emptying (EMPTY command; Dosing units only) functions. The preparation function is used to fill bubble-free and to rinse the exchange or dosing units if they have not been used for a long time. When this function has been carried out all the tubing and the cylinder will be filled with reagent.
3 Operation Enter the Volume of reagent which is to be dosed in during a rinsing cycle. The default value is the cylinder volume, i.e. the contents of one cylinder is dosed in during a rinsing cycle. You can also enter a different volume. Select the number of Cycles to be carried out during the preparation function. At least two rinsing cycles should be carried out in order to remove all the air bubbles.
3.8 Titrants Select the Dosing port via which the first cylinder contents are to be ejected during preparation and emptying. Enter the Dosing rates for all the ports to be used during the preparation and emptying functions for drawing in and ejecting the reagent. Lower rates should be entered for substances with higher viscosities. The maximum dosing rate and maximum filling rate for the dosing unit depend on the cylinder volume: Cylinder volume Max. rate 2 mL 6.67 mL/min 5 mL 16.67 mL/min 10 mL 33.
3 Operation 3.8.8 Monitoring the GLP test You can monitor the time interval after which a GLP test must be carried out again for the exchange or dosing unit. (A detailed description of the monitoring function using "Titer validity" as an example can be found in Section 3.8.4.) Open the dialog Exchange unit/GLP test or Dosing unit/GLP test. Enter the date of the last GLP test to have been carried out and activate the Monitoring checkbox. Enter either the GLP test interval or the date of the next GLP test.
3.9 Sensors 3.9 Sensors This section describes how you can draw up a list of the sensors used in the system. The following sensor data is stored in the list of sensors: • • • • • • • • • • Sensor name Sensor type Order number Serial number Comment Measuring input to which the sensor is connected.
3 Operation You can configure new sensors with [New] (see Section 3.9.1). Sensors can be removed from the list with [Delete]. Sensor data for intelligent sensors can be deleted even when they are just connected. The data will be entered in the list again the next time that the corresponding sensor is connected and the data read out. [Edit] opens the dialog for entering sensor data. 3.9.
3.9 Sensors 3.9.3 Editing sensor data Open the dialog Sensors/Edit by either configuring a new sensor (see Section 3.9.1) or selecting an existing sensor from the list and modifying it with[Edit]. Enter an unambiguous name for the sensor under Sensor. For ISE electrodes the ion whose concentration can be determined with the sensor is also shown. The Order number and Serial number are read out automatically in case of intelligent sensors. The data can be entered manually for non-intelligent sensors.
3 Operation Under Calibration data/History the calibration data, dates and times of the last ten calibrations are shown in the form of a table. Calibration data which have been determined automatically is shown in green, manually entered calibration data is shown in black and marked with (m). With [Graph slope] and [Graph pH(0)], or [Graph E(0)] you can open a graph in which the slope or pH(0) for pH electrodes or E(0) for ISE electrodes is plotted against the calibration date.
3.9 Sensors Open the dialog Edit sensor/Calibration interval and activate the Monitoring checkbox. Enter either the Calibration interval or Next calibration date. If the time interval or date is altered then the other parameter will be updated automatically. Select an Action to be taken when the time interval has expired. 3.9.
3 Operation 3.10 Device manager This section describes the configuration of the Touch Control, control devices (Titrando, USB Sample Processor etc.) and the connected peripheral devices. The installation of the hardware is described in the Installation Instructions for the Titrando. You should first connect all the peripheral devices and then configure them in the device manager. Open the dialog System/Device manager. The device list gives the name and type of every configured instrument.
3.10 Device manager 3.10.1 Configuring a new device Open the dialog System/Device manager. Use [New] to open the device selection window. Select the device type (Balance, Lab Link, Barcode reader, Titrando, Printer (Touch Control only), PC keyboard (Touch Control only), Sample Processor, Serial ports (PC Control only) or RS-232/USB Box (Touch Control only)). With the exception of the Titrando (maximum number 3) you can only log in one device of the same type.
3 Operation With Touch Control the Program version and Serial number of the Touch Control are shown. Under Switch off display enter the time after which the display illumination is to be switched off automatically when the system has not been used. As with the PC Control, the Control remote box connection is shown. The Device name of the PC Control or Touch Control is printed out in the standard report header. 3.10.
3.10 Device manager For the Measuring inputs the ADC type (Analog-Digital Converter) and Serial number of the measuring interface are shown. Select the Sensor type for the temperature sensor used at this measuring input. If you use an NTC sensor then you must set two further parameters that can be obtained from the technical specifications of the sensor: the nominal resistance at 25 °C (R (25 °C)) and the B value referring to measurements of the resistance at 25 °C and 50°C.
3 Operation Select a connection or a device and open the corresponding configuration dialog with [Properties]. The settings for the USB Sample Processor, the tower and the Swing Head are described on the following pages. For the MSB connections you can define when the request to carry out the preparation function (PREP command) for the connected doing devices is to be displayed. The preparation of the exchange or dosing unit is described in Section 3.24.2.
3.10 Device manager USB Sample Processor The Program version, the Serial number and the name of the current sample rack are shown for the USB Sample Processor connected. With [Adjustment data] you can access an overview of the EEPROM data of the USB Sample Processor. Attention! Do not modify these settings under any circumstances. This data is required by the service technician in case of positioning problems.
3 Operation • • • • head cannot move to any lower position than the value entered here (0 mm = upper lift stop position). Under Min. beaker radius you can enter the smallest permissible sample beaker radius for automatic and manual operation. This is also a safety setting in order to prevent a wide, fully equipped titration head from trying to enter a narrow sample vessel.
3.10 Device manager External position [Ext. pos. 1-4] can be used to assign shift and rinse positions that are valid for all four external positions. • • The swing rate is the rate at which the robotic arm is swung when moving to a rack position, a special beaker or an external position. In manual control and in the command MOVE this rate can be adjusted individually. The swing increment is the angle about which the robotic arm should be swung relatively to the momentary position.
3 Operation • • • Swing radius: The swing radius depends on the length of the robotic arm and together with the axial distance it is the most important parameter for moving accurately to a rack position. The required values can be found in the leaflet for the robotic arm. Rotation offset: The rotation offset is the offset from the center of the tower to the center of the robotic arm. Normally it does not have to be changed.
3.10 Device manager [Load] can be used to load new racks from a card. In PC Control the paths for Card 1 and 2 can be defined in the menu File/Preferences. These may be directories on a hard disk, a network drive or any removable storage medium. With Touch Control Card 1 or Card 2 can only be selected when it is actually in the card slot. The new rack has to be copied necessarily into a subfolder of "Files".
3 Operation • • • • the 1st calibration position then it is essential that the other calibration solutions are placed in the directly following rack positions. If special beakers are used for the calibration then there must be as many special beakers defined (see below) as buffers or standard solutions are required for the calibration. The special beakers do not need to be placed in rack positions that directly follow each other.
3.10 Device manager • • • • Rack position: Each special beaker can be assigned to any rack position. However, they should preferably be assigned to high rack positions so that sample series can be started with rack position 1. Rack positions that have been defined as special beaker positions are no longer available as sample positions. Work pos. Tower 1/2: A specific work position can be defined for each special beaker. See also Section 3.24.6.
3 Operation Open the list with the available racks with [Rack tables]. Select the desired rack and press [Edit]. Press [Adjust rack]. Press [Start] (not the green key). The rack is rotated so that rack position 1 is positioned in front of the tower. If a robotic arm is installed, it is swung to rack position 1. The lift then moves to the work position. The position of the lift can now be corrected with the arrow keys [u] and [v].
3.10 Device manager 3.10.6 Dosing Interface The devices at the MSB connections are listed in a table for the Dosing Interfaces that are connected. A stirrer and a dosing device are connected to MSB 1, a dosing device is connected to MSB 2. If the Dosing Interface is not connected, only the Device name and Comment can be edited. Select a connection or a device and open the corresponding configuration dialog with [Properties].
3 Operation Activate the checkbox Spooler in order that the Touch Control is not blocked by printing out a report so that you can continue working. Note! The Touch Control prints the reports with a fixed resolution of 300 dpi. If you are using a printer with a resolution of 360 dpi (or a multiple, e. g. Epson) then the text will be printed out somewhat smaller than with printers with a resolution of 300 dpi (or a multiple, e. g. Canon or HP). 3.10.
3.10 Device manager Touch Control: Under RS-232 select the RS-232 interface at the RS-232/USB Box which is used to connect the balance. Select the RS-232/USB Box in the device manager and open the list with the available RS-232 interfaces with [Edit]. Select the interface to which the balance is connected. Open the dialog with the port parameters with [Edit] and configure these. The settings on the balance must agree with these settings here. A description of the parameters can be found in the online help.
3 Operation 3.10.9 Bluetooth devices Connecting a Bluetooth USB adapter to the Titrando is described in the Installation Instructions for the Titrando. In the device manager you must configure the Bluetooth adapter used to connect the device. Look for all the devices within reach with [Find device]. If they are switched on, they are entered with status ok. Devices which are not switched on at the moment but once have been assigned to a printer or a RS-232 interface are entered with status not available.
3.10 Device manager Note! The spooler should be switched on to prevent the Touch Control or the printer from getting blocked (see properties dialog of the printer). In the report options, switch on the printing of the frame in order to accelerate the printing. 3.10.10 RS-232/USB Box / Serial ports You can adjust the parameters at the connected RS-232/USB Box or the RS interfaces of the PC respectively under Edit device/Port parameters. The parameters are described in the online help.
3 Operation 3.10.12 PC/LIMS module A machine-readable report containing all the data of a determination (PC/LIMS report) can be saved in a TXT file or sent to a terminal program or a LIMS via an RS-232 interface. The report is saved or sent either automatically at the end of a determination sequence (see Section 3.16.10) or manually with the [Print] fixed key (see Section 3.23.1). A detailed description of the contents of the PC/LIMS report is given in the Titrando PC/LIMS Report Guide.
3.10 Device manager Select the RS-232/USB Box in the device manager and open the list with the available RS-232 interfaces with [Edit]. Select the interface to which the report is to be sent. Open the dialog with the port parameters with [Edit] and configure these. The settings of the interface must agree with these settings here. A description of the parameters can be found in the online help. 3.10.
3 Operation 3.10.14 PC keyboard (Touch Control only) An external PC keyboard can be connected to a Titrando system with Touch Control to make the input of texts easier. Select the country-specific key occupancy under Keyboard layout. When the PC keyboard is selected the unambiguous identification of the manufacturer (Vendor ID) and the USB address will be shown automatically.
3.10 Device manager 3.10.15 Barcode reader A barcode reader can be connected to the Titrando system to read in sample data or other texts. When a barcode reader is connected to a Titrando system with Touch Control then it is automatically entered into the device list with default parameters. Barcode reader models which can currently be connected can be found on the Internet under www.titrando.com. Select the Barcode input target for the barcode character string.
3 Operation 3.11 File manager The file system of the Touch Control and PC Control has the following arrangement: Working memory Current method, current determination (incl. statistics), current sample data silo, current result silo, current system data (system settings, titrants, sensor data, device data, GLP data, common variables,...
3.11 File manager You can select the memory location to be used for the files. [Card 1] and [Card 2] are inactive when they cannot be accessed. With Touch Control the cards must be inserted before you open the file manager. [Shared memory] is only visible if an external file system is configured (requires 847 USB Lab Link, see Section 3.10.11). If only the internal memory can be accessed then the dialog System/File manager will be skipped.
3 Operation Note! In PC Control the file groups correspond to folders. Card 1 and Card 2 each have only one level for groups and folders. The file names must be unambiguous for all groups (folders) in a memory location. You should only manage the PC Control files with the file manager of the PC Control software. If you use Windows Explorer for this then there is the risk that you might no longer find the files in PC Control as the folder structure is not compatible.
3.11 File manager Open the Internal memory. The file groups in the internal memory are shown. You can arrange your files in the file groups. The file names must be unambiguous for each memory location, i.e. you cannot save a file in different groups with the same file name. From the list of files you can print out a list with all the files in these groups with the [Print] fixed key.
3 Operation 3.11.1 Copying files Select the file to be copied in the list of files and open the selection of the memory location with [Copy]. Select the memory location into which the file is to be copied. The file is copied. You can only select a memory location that can currently be accessed. If Card 1 or Card 2 cannot be accessed then you should exit the file manager and define the path for the card (for PC Control – see p.
3.11 File manager The following data is also shown: • • • • • • • User who saved the file for the first time. Date and time at which the file was saved for the first time. User who was the last to save the file. Date and time at which the file was saved for the last time. Version of the file. The version is increased by one each time that the file is saved under the same file name. The version is retained when the file is copied and loaded in a different system. The approximate Size of the file in kB.
3 Operation Select the memory location in which the file is to be stored under Memory. Methods can be saved in the Internal memory, on Card 1 or Card 2 or a shared file system (requires 847 USB Lab Link, see Section 3.10.11). All other files can only be stored on Card 1, Card 2 or a shared file system. You can arrange your files by storing them in different groups. Enter the Group in which the file is to be saved. You can also select the group from the list of existing file groups.
3.11 File manager Control the write protection applies to the folder defined for the card under File/Preferences/Paths. The following information about the card is shown: • • The Label of the card or data carrier which was entered when the data carrier was formatted or entered later under Properties in Windows Explorer. Storage capacity (total space), Used memory and Free memory for the card, or for the whole data carrier under PC Control. 3.11.
3 Operation Touch Control: Insert the card on which you want to make your safety copy in Card slot 1 or 2 of the Touch Control. PC Control: Select the directory or drive on which you want to make your safety copy under File/Preferences/Paths. You can now open the file manager and start the backup. Open the Card 1 or Card 2 memory location in the file manager. Start data storage with [Backup] and answer the query “Do you want to start the backup?“ with [Yes]. Only one backup can be stored on each card.
3.11 File manager • • • • • • • • • • • • • • Current determination data: all the data for the current determination and the current method with which the determination was carried out. Control: settings under control. User list under System settings/User administration and settings for each user.
3 Operation 3.12 GLP manager In the GLP manager you can document data for various GLP tests. The results of the automatic system tests carried out after START are also documented. You can also draw up a list containing the test tools which you use and enter a service interval for having routine maintenance carried out by a Metrohm service technician.
3.12 GLP manager With Touch Control (see example) the test is very comprehensive. The result of each test is shown in green if no error has occurred. If a result is shown in red then an error occurred when the corresponding test was carried out. Switch the system off and then on again. If the error still occurs pleased consult Metrohm Service. 3.12.2 Test tools You can create a list of test tools to be used in the tests in the GLP manager. The list already contains definitions of some test tools.
3 Operation 3.12.3 GLP tests for measurement and titration You can document the GLP tests for measurement and titration here. Open the dialog GLP manager/GLP tests HW/SW (HW = hardware, SW = software). Select [GLP test measurement] or [GLP test titration] according to which GLP test you wish to document. For both tests you can select or enter the Method with which the test is to be carried out. Only methods in the internal memory will be shown in the selection list.
3.12 GLP manager Open the dialog GLP test measurement/Test interval or GLP test titration/Test interval. Activate the Monitoring checkbox. Enter either the GLP test interval or the date for the Next GLP test. If the time interval or date is edited then the other parameter will be updated automatically. Select an Action to be carried out when the time interval has expired. The GLP test interval will always be monitored at the START of a determination. 3.12.
3 Operation Enter either the Validation interval or the date for the Next validation. If the time interval or date is edited then the other parameter will be updated automatically. Select an Action to be carried out when the time interval has expired. The validation interval will always be monitored at the START of a determination. You can enter a short note under System validation/Note (SOP), e. g. a summary of the SOP (standard operating procedure) according to which the system validation was carried out.
3.13 Common variables 3.13 Common variables Up to 25 device-specific, method-independent variables can be stored in the system. These variables can be calculated as CV01 to CV25. Common variables are always used when a result from one determination carried out with Method A is to be used in a determination carried out with Method B. Typical uses are in the determination of a Blank value or the content of a standard solution to be taken into consideration when calculating the content in a sample.
3 Operation Enter a name for the common variable under Name. Enter the Value and the unit of the common variable. The name and unit will be shown automatically when the value of the common variable is asked for with a REQUEST command (see below). Requesting a common variable during a determination sequence: Define a REQUEST command in the method as described in Section 4.13.3. Define the variable that you want to request (CV01 to CV25) under Common variable in the parameter dialog for the REQUEST command.
3.13 Common variables Automatic assignment of a result to a common variable, e. g. for a blank value determination : Define a CALC (calculation) command (see Section 4.5.1) in the method in which the result (e. g. the blank value) to be assigned to the common variable is calculated. This can also be the mean value of a multiple determination.
3 Operation 3.13.3 Monitoring the validity You can monitor the time interval after which the common variable must be assigned a new value. (A detailed description of the monitoring function using "Titer validity" as an example can be found in Section 3.8.4.) Open the dialog Edit common variables/Validity and activate the Monitoring checkbox. Enter either the time interval for the validity of the common variable or the date for the Next assignment.
3.14 Templates 3.14 Templates You can define system-specific templates for sample data, result calculations, remote lines, calibration buffers and the report header. You can use these templates when editing the corresponding data. Open the dialog System/Templates. 3.14.1 Sample identification list You can create a system-specific list with templates for sample identifications.
3 Operation The dialog in which you can enter the templates for sample identifications is opened automatically with [New]. For an existing template this dialog can be opened with [Edit]. Existing sample identifications can be removed from the list with [Delete]. Exit the dialog with [Back] and activate the Use sample identification list checkbox so that you can select from the templates when entering the sample data. 3.14.
3.14 Templates The dialog in which you can enter the templates for sample identifications is opened automatically with [New]. This dialog can be opened with [Edit] for an existing template. Existing sample identifications can be removed from the list with [Delete]. Enter the Identification for the sample assignment. You can also select an identification from the sample identification list (see Section 3.14.1). You can enter an * as a wildcard at the beginning or end of the character string.
3 Operation 3.14.3 Custom results templates Templates can be created for editing result calculations in the methods; these can be loaded when editing CALC commands. Open the dialog Templates/Custom result templates. With [New] you can define new templates. Existing templates can be removed from the list with [Delete] or altered with [Edit]. Use [New] to open the edit dialog for a new result template.
3.14 Templates 3.14.4 Input lines Binary patterns can be defined for scanning remote lines with the SCAN command (see Section 4.11.1) during the determination sequence; these can then be selected when editing the parameters. Open the dialog Templates/Input lines. You can define new templates with [New]. Existing templates can be removed from the list with [Delete] or edited with [Edit].
3 Operation To input the binary pattern please consult the online help. 3.14.5 Output lines Binary patterns can be defined for setting remote lines with the CTRL command (see Section 4.11.2) during the determination sequence or in manual operation (see Section 3.24.5); these can then be selected when editing the parameters. Open the dialog Templates/Output lines. You can define new templates with [New]. Existing templates can be removed from the list with [Delete] or edited with [Edit].
3.
3 Operation 3.14.6 Custom calibration buffers You can define five of your own calibration buffers which can then be used for calibration with automatic buffer recognition. The buffer series can be selected in the CAL (calibration) command as the Custom buffer series (see Section 4.7). Open the dialog Templates/Custom calibration buffers. Enter the pH of the first buffer under Buffer 1. Use Temp.table to open the temperature table for this buffer.
3.14 Templates 3.14.7 Report header You can enter a text here (max. four lines each with 46 characters) which will always be printed out in front of the standard report header (see Section 3.23). Enter the text for your Report header. If you want to print out the Metrohm logo to the right of the text then activate the Print logo checkbox and select Metrohm logo in the selection list. If you wish to print your own logo in the report header select Custom logo.
3 Operation Confirm with [Generate]. In PC Control the logo can be used directly; for Touch Control the file CustomImage.bin is generated in Card 1 (see menu Preferences). Save this file onto a memory card, insert it in Touch Control card slot 1 and load the file. This is done by selecting the Touch Control under Device in the menu System/Diagnosis/Software update. In the selection list Update Type, select the item System file and confirm with [Continue].
3.14 Templates • • • • • 106 Streaming potential: The streaming potential is the difference between the voltages measured in stirred and unstirred solution. Drift: For each buffer, the drift in stirred solution is determined. The sum of these values is compared with this value here. Slope min.: Minimum slope of the pH electrode. Slope max.: Maximum slope of the pH electrode.
3 Operation 3.15 Loading methods The sequence of a determination is defined in the method. In the Load method dialog you can load saved methods or method templates for creating new methods. 3.15.1 Loading a method Methods can be saved in the internal memory, on Card 1 or Card 2 or a shared file system (requires 847 USB Lab Link, see Section 3.10.11).
3.15 Loading methods Select the group Examples and open the file list for this group with [Show files]. With [Show all] you can open the list of files containing all the methods in the selected memory. Select a method from the list, e. g. Determination of HCl and [Load] it. When the file has been loaded the program will jump automatically to the main dialog. If the method contains a Note which is displayed when the method is loaded then this can be closed with [Continue].
3 Operation The individual templates are described on the following pages. The commands in the method templates have standard parameters. These standard parameters are suitable for most titrations. Note! If you would like to test a new titration method then select the Dynamic titration pH or U template. Dynamic titration is suitable for practically all standard applications and you only have to adapt individual parameters in special cases.
3.15 Loading methods The following method templates can be selected: Method template 110 Command sequence Application Dynamic Titration pH DET pH (dynamic titration) CALC REPORT (result report and titration curve) Dynamic Titration U DET U (dynamic titration) CALC REPORT (result report and titration curve) Dynamic reagent addition, for rapid equivalence point titrations, large volume increments in the flat part of the curve; small increments near the EP, many measuring points near the EP.
3 Operation Method template Command sequence Application STAT pH with pretitration SET pH (endpoint titration) WAIT STAT pH (Titration with holding the measured value constant) EVAL RATE (Rate evaluation) CALC REPORT (result report and titration curve) Titration to a predefined control point. The control point is kept constant by continuous reagent addition, e. g. for determination of enzyme activity.
3.15 Loading methods Method template Command sequence Application SP Method rinse sample beaker MOVE (rotate rack) LIFT (move lift to work position) STIR WAIT STIR SUBSEQ (aspirate and rinse in sample beaker) SUBSEQ (End sequence) Titration with the USB Sample Processor. The WAIT command must be deleted and replaced by a titration, a CALC and a REPORT command.
3 Operation 3.16 Editing parameters Here you can define and edit the method commands which are processed successively during a determination. From the main dialog use [Edit parameters] to open the list of commands for the current method. If you have loaded a method (see Section 3.15.1) then the list of commands will already contain a sequence of method commands. If you have used [Empty method] to create a new method (see Section 3.15.2) then the list of commands will still be empty.
3.16 Editing parameters commands and parameters can be found in Section 4. The input range for all parameters can be found in the online help. Select the command in the list for which you want to edit the parameters and open the edit dialog with [Edit command]. In the example shown the command DET pH has been selected. The command number, the command name and the command comment are always shown in the first row. The comment can be edited in the input field.
3 Operation 3.16.2 Insert command A method may contain a max. of 99 commands. You can use [Insert command] to insert a new method command in front of the selected line. In the example shown a new "empty" method is being edited. Use [Insert command] to open the dialog Sequence/Insert command. The method commands are arranged in different groups. An overview of all commands and parameters can be found in Section 4. The individual commands are also described in the online help.
3.16 Editing parameters 3.16.3 Method options Method options are settings which apply to the method as a whole and not to an individual command. For example, you can switch Statistics on and off, Show direct parameters on and off, automatically save the determination at the end of the run, sign a method, enter a Note and make the settings for sample data input. Open the dialog Sequence/Method options. [Properties] accesses an overview of the properties of the current method.
3 Operation • • • • User: Enters the identification of the user who signs. In the overview of the method properties the name of the user appears as given under User admin./Edit under Full name. If no complete name has been entered there then the identification appears in the overview of the method properties. Password: Enters the password. Reason: Selects the reason for the signature. Under Login options/Reasons (see Section 3.7.7) the list of reasons can be defined by users with Administrator rights.
3.16 Editing parameters [Cancel] rejects the entries and returns to the overview of the method properties. [Delete signature] deletes all the signatures to the method and returns to the overview of the method properties. The method then has the status "Saved". 3.16.4 Statistics If you want to statistically evaluate certain results, which have been calculated during the determination sequence then you must make the following settings: Activate the Statistics checkbox.
3 Operation 3.16.6 Sample data In the method you can adapt the label of the sample identifications 1 and 2 which are shown in the main dialog. You can also define the Sample size unit or a Fixed sample size. The sample size can then no longer be edited in the main dialog. If you define Sample size limits then these will be monitored during the determination after START and at the end of the determination.
3.16 Editing parameters Only Identification 1 is shown with the title "Charge". The fixed sample size "10 mL" is shown and cannot be edited. You can also define the limits for the sample size which will then be monitored in the determination sequence. Open the dialog Sample data/Sample size limits and activate the Monitoring sample size limits checkbox. Enter a Lower limit and an Upper limit for the sample size.
3 Operation 3.16.7 Start and stop options Under Method options/Start/Stop options you can switch various start and stop options on and off. Under [Start options] you can switch off the Method check, which is carried out automatically after the START of a determination. This avoids delays after the START. The Method check verifies whether all devices, titrants and sensors which are necessary for the run are present and whether monitoring intervals for the titrants and sensors used have expired.
3.16 Editing parameters • • • Manual termination with the [STOP] fixed key Termination because of an error Termination by remote signal via the Control remote box If the checkboxes Pumps off and Stirrer off are activated then, when a method is stopped, all the connected pumps and stirrers will be switched off. Under Set remote lines you can enter a binary pattern or select a signal from the templates. The templates are defined under System/Templates/Output lines.
3 Operation 3.16.9 Properties The properties of the current method are shown under Method options/Properties. An explanation for the individual entries can be found in the online help. The method shown as the example has already been saved twice (version 2). In comparison to the stored version 2 further parameters have been edited, so that the Method status is not saved but modified.
3.16 Editing parameters Under Memory select the memory location in which the determinations are to be stored. Determinations can only be stored on Card 1 or Card 2 or a shared file system (requires 847 USB Lab Link, see Section 3.10.11). Enter the Group in which the determinations are to be stored.
3 Operation 3.16.11 Save method You can save the current method in one of three memories (see Section 3.11). From the main dialog use [Edit parameter] to open the command list for the current method. If the use of direct parameters has been switched on (see Section 3.16.5) then the direct parameter list will be opened; the method can also be saved from here. Use [Save method] to open the dialog for selecting the memory, file group and file name. If you have created a new method (see Section 3.15.
3.17 Control 3.17 Control This is where various settings for a determination run or for processing a series of samples are made. If you are working with login (see Section 3.7.7), then you can use [Logout] in this dialog to log out of the system The login dialog will then be shown. From the main dialog open the Control dialog. The Sample number is primarily used for documentation. Each time that a determination is started with START it is increased by one.
3 Operation Load the last determination in the sample series that you have previously saved (see Section 3.18.6). The method used and the current statistics data will also be loaded together with the determination. The statistics button under Control and the statistics counter will have the same status as they had before the interruption to the sample series. Continue with the processing of the sample series. You can view the statistics overview under Results/Statistics (see Section 3.21).
3.17 Control 3.17.3 Autostart The autostart function is used for processing a sample series. If the Autostart checkbox is activated then a new determination will be started automatically when a determination has ended until the set Number of autostarts has been reached. The number of autostarts can also correspond to the number of samples defined in the sample data silo (see Section 3.19.3).
3 Operation 3.18 Results and more determination data The most important details of the current determination (method used to carry out the determination, name of the determination, determination time), the calculated results (result name and result with unit) and the raw data (e. g. endpoints or final measured values) are shown under Results. From the main dialog open the Results dialog.
3.18 Results and more determination data 3.18.1 More determination data Under Results/More determination data a list containing all the method commands which produce raw data (titrations, measurements, calibrations and monitored dosing) and evaluations (EVAL commands) is shown. Open this list with [More determination data]. Under View data the details (raw data and variables) for the selected command are shown. Select a command and press [View data].
3 Operation The [Calibration data] and [Titrant data] buttons are only present when the determination has been loaded. With [EP details] you can view details of the endpoints. This button is only available for the titration modes DET, MET, SET and KFT. With [MP list] you can open the list of measuring points of a titration, measurement or monitored dosing. List of measuring points The list of measuring points is displayed in the dialog View data/MP list. Press [MP list].
3.18 Results and more determination data The individual variables are described in Section 4.5.7. The ERC (Equivalence point Recognition Criterion) is a measure of the size of the jump in the titration curve. The ERC found is compared with EP criterion defined in the method for the evaluation of the titration curve (see Section 4.1.1). The ERC is therefore an important quantity if you have to adapt the parameters for the evaluation of the equivalence points.
3 Operation With [Details] you can show the unambiguous identification number of the message, the time when the message was produced during the run and the message text for the selected message. 3.18.3 Local common variables The [Local common variables] button in the dialog Results/More determination data is only present when the determination has been loaded. In this dialog the list of common variables as they were at the time when the determination was carried out is shown.
3.18 Results and more determination data The following data is shown for each determination: • • • • • • • • The user who was logged in when the determination was carried out is shown under User. If you are working with login and password protection (see Section 3.7.7), you can be certain that only authorized users can carry out determinations. Under Sample number the sample number entered at the end of the determination under Control is shown.
3 Operation A determination can be signed up to three times at each level. The devices used for the determination sequence are shown for each determination. This means that you can document the devices used to carry out each determination. • • • • Touch Control with program version (P) and serial number (S) or PC Control with program version (P) and serial number (S) of the dongle (authorization plug). If no dongle is connected then "Demo version" will be shown. Control device (Titrando etc.
3.18 Results and more determination data determination are deleted and you return to the properties of the determination. 3.18.5 Save determination You can save the current determination on Card 1, Card 2 or a shared file system (requires 847 USB Lab Link, see Section 3.10.11). In this way you can store all the data of a determination. If you wish to save every determination then you can use the function Save automatically (see Section 3.16.10).
3 Operation Use [Show all] to open the list of files containing all the files or [Show files] to open the list of files for the selected group. Only determination files will be shown. In the following example the list of files for the determinations stored under Examples is shown. These determinations are stored on Card 1 (PC Control) and on the supplied data card with the examples of methods (Touch Control). The selected file is loaded with [Load].
3.18 Results and more determination data Above the list the sorting criterion together with the total number of determinations is shown. Each line corresponds to a determination. The selected file is loaded with [Load]. You can remove the selected file from the list of files with [Delete]. Under Browser/Properties you can select the sorting criterion as well as the data to be shown in the list. You can also use filters on the list. Open the dialog with [Properties].
3 Operation Select a filter criterion under Filter and enter the corresponding text or the time range or the range of values in the lines below. The filter can be applied to empty fields as well, for example, if no sample identification has been entered. In this case, select only the desired filter criterion and leave the fields below empty. Only one filter criterion can be active at a time. Only those determinations which meet the filter criterion will be shown in the Browser file list. 3.18.
3.18 Results and more determination data The settings for the curve view are saved separately and systemspecifically for each mode. They apply to the curve view under results as well as to the live display (see Section 3.20.4). 3.18.
3 Operation calculations. If a result of the variable TITER is assigned in a calculation then the titer of the "new" titrant will also be overwritten. Note! An alteration of the calibration data under System/Sensors (see Section 3.9.4) cannot be taken into account in a recalculation. A change of the sensor in a method for a titration or measurement also has no influence on the measured data. The fact that a determination has been recalculated is shown under More determination data/Properties (see Section 3.
3.18 Results and more determination data 3.18.9 Export (PC Control only) You can export results, lists of measuring points and sample data of the current determination to Excel or as a text file. Open the export dialog under File/Export.... • Data for export: Activate the checkboxes for the data you wish to export. • Excel: Click on Excel if you want to export the data to an Excel table. Press [...] and select the program file EXCEL.EXE in the installation directory of Microsoft Office.
3 Operation 3.19 Sample data If you wish to process single samples then you can enter the identifications and sample sizes for the current sample directly in the main dialog. You can also program an automatic sample data request during the determination sequence with a REQUEST command. If you are processing sample series then it is a good idea to use the sample data silo.
3.19 Sample data is shown in the main dialog, but can be edited. A fixed sample size cannot be entered in the main dialog. You can also define sample size limits in the method which will be monitored during the determination sequence (START of the determination and at the end of the determination) (see Section 3.16.6). Note! The sample size limits are not monitored during the input of the sample data in the main dialog. 3.19.
3 Operation 3.19.3 Sample data silo If you would like to use the sample data silo then you must activate the corresponding checkbox under Control. With PC Control you can also enter the sample data when the sample data silo has not been activated. You can open and close the table in the menu View. With Touch Control the sample data silo for the sample data input must be activated.
3.19 Sample data Click on Action in the title line of the sample data silo. You can use Insert line to insert a new silo line in front of the selected line, delete the selected line with Delete line and clear the whole of the current silo with Delete all silo lines. The settings under Sample data silo/Properties are retained. You can use Load sample data silo to open the dialog for loading a sample data silo file and Save sample data silo to open the dialog to save the current sample data silo.
3 Operation two further columns can be shown. The columns to be shown is defined under Sample data silo/Properties (see p. 149). 1 Note! Sample data silo files can be exchanged between PC Control and Touch Control as their contents are identical. With [Edit] you can open the dialog in which the data for the selected line is to be entered. [Delete] is used to delete the selected silo line. With [Insert line] you can insert an empty silo line in front of the selected silo line.
3.19 Sample data You should now enter the sample data, irrespective of whether you are using PC Control or Touch Control. Under Method you can select the name of the method with which the sample is to be processed. You can use Sample data silo/Properties to define the Method memory (internal memory, Card 1, Card 2, Shared memory) from which the method is to be loaded. You can also enter the method name. If no method is entered then the current method will be used.
3 Operation list or entered directly. You can also send the sample size from a connected balance (see Section 3.10.8). If you have defined a sample size unit (see Section 3.16.6) then this will be ignored in the sample data silo. The sample size unit entered in the sample data silo will always be used. If you have defined a fixed sample size (see Section 3.16.6) then this will be written into the corresponding silo line when the method is opened.
3.19 Sample data You can disable editing the sample data in the sample data silo. This is a good idea when the sample data silo has been filled and you wish to prevent data from being altered while the silo is being processed. Display options (Touch Control only) Open the dialog Properties/Show options and deactivate the checkboxes for the sample data you do not want to use. These will then no longer be shown in the edit dialog for the individual samples.
3 Operation Save sample data silo Sample data silo files can only be saved on Card 1, Card 2 or a shared file system (requires 847 USB Lab Link, see Section 3.10.11). Open the selection Load/Save in the dialog Sample data silo. Touch Control: If no card is inserted or no external file system is shared, then the [Save] button is inactive. Open the dialog Save. The procedure for saving a file is described in Section 3.11.
3.20 Determination sequence 3.20 Determination sequence This section provides a description of how to carry out a determination, i.e. how to process a single sample or a sample series. The determination sequence is defined in the method. When a determination is started the current method is processed line by line. The current sample data is used for calculations. 3.20.
3 Operation 3.20.2 Processing a sample series You can use the following functions when processing sample series: Statistics for multiple determinations: Activate the Statistics checkbox in the method under Options Method and enter the Number of samples whose results are to be used for the statistical calculations. You can carry out the determinations individually or use the sample data silo for entering the sample data (see below).
3.20 Determination sequence data silo line is copied into the determination file and the line in the sample data silo is deleted. In case results of the determination are saved in the result silo they will be copied into the result silo at the end of the determination (see Section 3.22). If you have switched on the use of the sample assignment table (see Section 3.14.
3 Operation With [Results] you can open the results display. The data for the method commands which have already been carried out will be shown. The Results dialog and its subdialogs will not be updated during the sequence as long as they are open. If you want to view the most recent results you must exit the dialog and then reopen it. With [Edit parameter] you can edit the live parameters, i.e. the method parameters which can be altered while a sequence is being processed (see Section 3.20.6).
3.20 Determination sequence You can choose whether you would like to display the curve with the measured values to the right of it (default setting), only the curve (larger, fills the whole display), only the measured values (large) or the curve with the sample data to the right of it. You can alter the appearance of the curve with [Curve options] (see Section 3.18.7). The settings for the curve display are stored separately and system-specifically for each mode.
3 Operation 3.20.5 Main dialog "live" The appearance of the main dialog changes slightly when a determination has been started. The sample data can also be entered "live", i.e. while a determination is being carried out (see Section 3.19.1). In calculations the sample data which has been entered in the main dialog at the time when the calculation is carried out (CALC command) is always used. No device-specific settings can be carried out "live"; this is why the [System] button is not available.
3.20 Determination sequence 3.20.6 Live parameters Certain method parameters can be edited while a determination is being carried out. Open the Edit parameter dialog while a determination is currently being carried out. The [Edit command] button is active for a command in which live parameters can be edited. The sequence, i.e. the sequence of commands, cannot be altered. This is why the [Delete command] and [Insert command] buttons are inactive.
3 Operation The edited parameters are immediately taken into account in the determination sequence. However, for example, if you alter the start conditions after the start volume has already been added then these alterations will only be taken into account the next time that the method is started. Note! If the sample data silo is used and a different method is loaded for the next sample then the live alterations will be lost.
3.21 Statistics 3.21 Statistics In the Results dialog you can open the statistics overview of a multiple determination with [Statistics]. A maximum of nine results calculated in a single determination can be statistically evaluated. A statistics series can contain a maximum of 20 determinations, i.e. samples.
3 Operation 3.21.1 Statistical information about the result Select a result and press [Details]. The name of the result and the variable for the mean value (in this example SMN1) are shown under Details for each result (see Section 4.5.1). The Mean value and the absolute (s +/-) and relative (s rel) standard deviation are also shown above the list. The number of individual results used for the calculation of the mean value is shown to the right of the mean value.
3.21 Statistics 3.21.2 Delete statistics data You can delete the whole statistics data manually under Control with [Delete statistics]. The statistics data is deleted automatically in following cases: • • when the actual statistics counter (number of processed samples) is the same as the preset number of determinations used for the statistics. The maximum value of the statistics counter is defined under Sequence/Method options. when a method is loaded with [Load method].
3 Operation 3.22 Result silo The result silo is ideal for providing a clear overview of the results carried out, for example, on a particular day. You can store the results of up to 200 determinations. A maximum of nine results from a single determination can be stored in the result silo. As the display is not large enough to show all the data at the same time, it is a good idea to print out the result silo (see Section 3.23).
3.22 Result silo 3.22.1 Properties of the result silo Under Result silo/Properties you can choose the criteria according to which the list is to be sorted and the data to be shown for each determination. Open the dialog with [Properties]. Select the Contents of Column 1 and Column 2. In Column 1 you can display the sample data (Identification 1 or 2, or sample size), determination time, method, the name of the result or the user. In Column 2 you can select the result to be shown.
3 Operation Select a filter criterion under Filter and enter the corresponding text or the time range or the range of values in the lines below. The filter can be applied to empty fields as well, for example, if no sample identification has been entered. In this case, select only the desired filter criterion and leave the fields below empty. Only one filter criterion can be active at a time.
3.22 Result silo 3.22.2 Saving and loading the result silo Save result silo Result silo files can only be saved on Card 1, Card 2 or a shared file system (requires 847 USB Lab Link, see Section 3.10.11). Open [Load/Save] in the dialog Results/Result silo. Touch Control: If no card is inserted or no external file system is shared, then the [Save] button will be inactive. Open the Save dialog. The procedure for saving a file is described in Section 3.11.4.
3 Operation 3.23 Print In principle there are two ways of printing a report in Touch Control and PC Control: • • Manual printout with the [Print] fixed key (see below). Printout during the determination sequence with a REPORT command (see Section 4.6). By using the PC Control software you have the additional possibility to generate reports directly as PDF file. The settings are described on page 175.
3.23 Print The selected report can be printed out with [Print]. With [Edit] the parameters for the printout can be edited for some reports. The [Send] button is only active when PC/LIMS report has been selected. [Method reports] opens the list of reports for the current method. The list containing all the reports about the system-specific data is opened with [System reports]. If the [Print] fixed key is used then the reports will always be printed out with the default settings.
3 Operation Open the dialog for the report configuration with [Report options] in the Print dialog. In the Report header the type, serial number and program version of the software (Touch Control or PC Control), the device name which you can enter in the device manager for Touch Control or PC Control, and the printout date with time zone are printed out.
3.23 Print The following reports can be printed out with the [Print] fixed key: Report Contents Print / More reports Results (current determination) Statistics Sample data 170 Result report Determination properties, sample data, raw data, i.e. endpoints, final measured values, results of evaluations (EVAL), calculated results, short statistics, messages produced during the determination. Curve The settings for the curve print-out are adopted from the display.
3 Operation Result table Report Contents Sample data silo Sample data silo properties, landscape format, table with all sample data entered in the sample data silo. Result silo Result silo properties, landscape format, table with all results stored in the result silo. Print / More reports / Method reports Current method Method sequence Method properties, list with all method commands. Parameters full Method properties, method options, all method commands with all their parameters.
3.23 Print Titrants Sensors Device 172 Report Contents User list Context-sensitive only; list of all the users defined in the system under user administration. This report can only be printed out by the administrator. Login options Context-sensitive only; from the edit dialog for login options. List with all login option settings. This report can only be printed out by the administrator. Titrant list List of all the titrants configured in the system.
3 Operation Report Contents All device properties Properties of all the devices configured in the system. Device properties Context-sensitive only; from edit dialog for the device. Properties of the device which is currently being edited. GLP manager GLP data All data stored in the GLP manager. Common variables Common variable list List of all the common variables defined in the system. All common variable properties Properties of all the common variables defined in the system.
3.23 Print Note! Some tables (statistics overview and sample data silo) are always printed out in landscape format, as otherwise the data could not be printed out on a single page. For PC Control you must select the Windows-specific Printer setting: portrait, as printout in landscape format is automatic. 3.23.
3 Operation 3.23.2 Printing PDF reports Open the edit menu under File/Printer.... • Printer for report prints: Selecting the printer for the report output on paper from the list of all printers installed on the PC. • Generate PDF report: Activate this checkbox so that you are able to make the following settings for the PDF report. • Path for PDF file: The default setting for the PDF report is a separate folder "PDF_report" in the PC Control installation folder. You can select a different path with [...].
3.24 Manual control 3.24 Manual control The following functions are available in the manual control: • • • • • • Measuring Dosing Controlling a USB Sample Processor Manual titration Stirring Requesting and setting remote lines The manual control of devices that are not being used in the sequence is also possible during a determination sequence (BUSY). The dialog for manual control is opened with the [Manual] fixed key.
3 Operation Touch Control: Touch the [Manual] fixed key. Selecting the control device If you have connected several control devices then, after selecting the function, possibly you have to select the control device (Titrando, USB Sample Processor etc.) that you want to work with. The respective device names are displayed. The name and further settings are configured under System/Device manager (see Section 3.10).
3.24 Manual control 3.24.1 Measure Select the [Measure] function in the Manual control dialog. First select the sensor to be used for the measurement. All the sensors defined under System/Sensors will be shown. Select the Measuring input to which the sensor is connected. Select the Measuring mode. The measuring modes that are suitable for the connected sensor will be shown. If a temperature sensor is connected then the temperature will be measured automatically.
3 Operation 3.24.2 Dosing In the dialog Manual control/Dosing you can dose manually and prepare or empty dosing devices. You can also check which dosing devices are connected and which exchange or dosing units are attached. Select the [Dosing] function in the Manual control dialog. If several dosing devices are connected to a control device then the dialog for selecting a dosing device will be opened.
3.24 Manual control For type 8XX dosing devices with an intelligent exchange unit or dosing unit the data stored on the data chip will be displayed. For type 6xx or 7xx dosing devices you can select a titrant from the titrants configured under System/Titrants. Only those titrants which are suitable for use with the corresponding type of dosing device will be shown in the selection list, i.e. dosing units for Dosinos and exchange units for Dosimats. The cylinder volume is checked when dosing is carried out.
3 Operation selected then the dosing rate cannot be altered while dosing is taking place. Enter the Filling rate. The rate should be reduced for viscous liquids. The maximum filling rate depends on the cylinder volume of the exchange or dosing unit used (see Section 3.8.6). You can carry out manual dosing with [Dose]. When a cylinder volume has been added, the dosing cylinder will be refilled automatically. You can refill the dosing cylinder with [Fill]. The shown volume will be reset to 0.0000 mL.
3.24 Manual control The specified volume is shown above the volume that is already dosed. If the Fill automatically checkbox is deactivated then the button [Fill] is available additionally. [Stop] is used to stop the addition. You can use [Hold] to interrupt the addition and continue it with [Continue]. Fill You can fill the dosing cylinder manually with the [Fill] function. The piston and valve positions are shown during the filling process. Filling is carried out at the maximum filling rate.
3 Operation Example: Exchange unit Example: Dosing unit Empty The [Empty] function can only be carried out with dosing units. The Empty function empties the cylinder and all the tubing of the dosing unit. The parameters defined under System/Titrants for preparing the dosing unit and the tubing parameters are used for emptying (see Section 3.8.6). You can use the empty and prepare functions to change easily the reagent of a dosing unit without coming into contact with chemicals.
3.24 Manual control 3.24.3 Stir All the connected stirrers can be controlled manually. Select the [Stir] function in the Manual control dialog. The connection (MSB 1...4) and (in brackets) the stirrer type are shown for each Stirrer. You can increase the stirring rate with [u] or [+] and decrease it with [v] or [-]. The stirring direction changes as the sign changes ("+" means counterclockwise and "–" means clockwise when seen from above).
3 Operation 3.24.4 Manual titration Manual titrations can be carried out in the pH, U (mV), Ipol (mV), Upol (μA), concentration and T (°C) measuring modes. Select the [Manual titration] function in the Manual control dialog. Select a Dosing device. With intelligent exchange or dosing units the Titrant contained in the exchange or dosing unit will be displayed. With "non-intelligent" units the cylinder volume will be shown. Select a Stirrer.
3.24 Manual control ("+" means counterclockwise and "–" means clockwise when seen from above). You can carry out manual dosing with [Dose]. The dosing cylinder will be refilled automatically when a cylinder volume has been added. Dosing will be carried out for as long as long as the [Dose] button is pressed down. The addition is always dynamic, i.e. dosing will be carried out quicker and quicker until the maximum dosing rate has been reached (starting with 1 mL/min and then doubling the dosing rate every 1.
3 Operation 3.24.6 USB Sample Processor With a connected USB Sample Processor you can trigger any movement or function manually. You can end lift and rack movements prematurely with [Stop]. In the dialog Manual control select the function [Sample Processor]. [Rack reset] must be pressed if you have positioned a new rack or have carried out alterations to the current rack table in the device manager without having them transferred directly afterwards to the USB Sample Processor (see Section 3.10.5).
3.24 Manual control The two arrows [u] and [v] can be used to move the lift directly up and down for as long as the button is kept pressed down. The current lift position is shown continuously. [Previous] and [Next] rotates the previous or next rack position such that it is placed in front of the selected tower or robotic arm. Pump Activate [Pump] in order to access the control of the pumps. You can now turn the pumps on and off. Two pumps that can be controlled are always shown for each tower.
3 Operation Special beaker: An individual specific work position can be defined for each special beaker. The shift, rinse and special position of the affected tower are taken from the general rack positions. External position (with Swing Head only): With the external positions a specific work position can be defined for each of the four positions. A shift and rinse position can only be defined for all four external positions together. No special position can be assigned here.
3.24 Manual control Select the required lift position and press [Assign]. Move to rack position [Rack pos.] accesses the selection of the special beaker positions. Select the required entry under Rack position or enter an absolute rack position and press [Start]. The required rack position is moved to. Only those special beakers will be offered for selection that are defined in the current rack table (see Section 3.10.5). The shift rate and the shift direction of the sample rack can be changed here.
3 Operation The [s] and [t] arrows move the robotic arm to the left or to the right, respectively. As soon as you release the arrow key the current angle position will be shown. With [Assignm. Ext. pos.] you can now assign a swing angle to the individual external positions. Under Move to ext. pos. you can select the required external position directly or you can also enter a swing angle. Pressing [Start] moves to the corresponding angle position.
3.
4 Parameters 4 Parameters All the parameters for the method commands, from which a list of commands can be constructed, are explained in this section. How you can insert an individual command in the list of commands is described in Section 3.16.2. The way of selecting a command from the list and editing it is described in Section 3.16.1. With many numerical inputs you can also enter a special value (e. g. off) or a result that has previously been calculated (e. g. R1) instead of a number.
4.1 Titrations Note! As the reagent addition in DET depends on the measuring data, the titration curve should not vary too much from an S-shaped curve. • Monotonic equivalence point titrations (MET) with reagent addition at constant volume increments for titrations with relatively high signal variations or suddenly occurring potential jump and for slow titrations or slowly responding electrodes. Measured value acceptance is drift-controlled (equilibrium titration) or after a waiting period.
4 Parameters • Karl Fischer titration (KFT) for determining the water content by the Karl Fischer method with automatic pre- and post-conditioning. A typical feature of the Karl Fischer titration is the controlled reagent addition, which depends on the control difference (current measured value – endpoint), with the aim of reaching the measured value given as being the predefined target endpoint as quickly and accurately as possible. Overtitrating is avoided to a great extent.
4.1 Titrations • Endpoint titrations while holding the measured value constant. pH STAT is the most frequently used titration. A reagent is used to dose to a preset measured value (control point). This control point is kept constant by titrating the reaction product continuously with the reagent. The STAT titration keeps the control point constant until the preset stop condition has been reached. The STAT titration is used, for example, in enzymatic analysis.
4 Parameters 4.1.1 Dynamic equivalence point titrations (DET) and monotonic equivalence point titrations (MET) For equivalence point titrations (DET, MET) the parameters are identical except for a few exceptions. Both modes are described together here.
4.1 Titrations The User-defined Parameters differ for dynamic equivalence point titrations (DET) and monotonic equivalence point titrations (MET). User-defined titration parameters for DET and MET • • DET: Measuring point density (d): A small value means small volume increments, i.e. a high measuring point density. The curve then shows all the finest details which also include noise; this could cause unwanted equivalence points to be found. A larger value, i.e.
4 Parameters Note! A constant measured value is often only achieved after a certain time, as mixing and possibly the reaction itself require a certain time. The response time of an electrode can also increase with time, i.e. reaching a constant measured value takes longer and longer. In such a case drift-controlled measured value acceptance is particularly advisable, as the measured values are only accepted when equilibrium has almost been achieved. • Waiting time min.
4.1 Titrations The conditions for terminating the titration are defined under Stop conditions: • • • • • Stop volume (d): Stops when the preset volume (including start volume) has been added since the start of the titration. The stop volume should be adapted to suit the sample weight or the titration vessel size. Stop measured value (d): Stops when the preset value for a measuring point has been exceeded or undercut since the start of the titration.
4 Parameters When the list is opened for the first time you will see that it already contains a window which covers the whole measured value or volume range. You can add and edit new windows with [New]. The selected window can be removed from the list with [Delete]. You can use [Edit] to adapt the upper and lower limits for the selected window. All calculable variables can also be applied as result variable R1…R9. This means that you have to define the results in a preceding CALC command.
4.1 Titrations the last (only the last EP to be found), ascending (only EPs with a positive titration curve slope), descending (only EPs with a negative titration curve slope). Only one equivalence point will be recognized per window. The numbering of the equivalence point (EP) is determined by the numbering of the window (e. g. EP2 in window 2), so that even if EPs are missing the calculations will still be carried out with the correctly assigned EP volumes. U/mV U/mV EP window 2 EP window 1 u.
4 Parameters pH Inflection point VE V/mL Fig. 4.7: Tubbs method for determining the equivalence point The figures shows that the evaluation also requires measuring points after the equivalence point too. For the recognition of the EPs found the set EP criterion is compared with the ERC (Equivalence point Recognition Criterion) found. The ERC is the first derivative of the titration curve combined with a mathematical function which is more sensitive for flat jumps than for steeper ones.
4.1 Titrations In the example shown an EP criterion of 20 would make sense if only the first equivalence point is to be recognized. Evaluation and equivalence point criterion in the MET mode The equivalence points (EPs) are localized by a procedure based on the Fortuin method which has been adapted by Metrohm for numerical methods. A search is made for the largest measured value alteration (∆n).
4 Parameters The parameters for Control device, Sensor, Dosing device and Stirrer are described in Section 4.1.5. Titration sequence for DET and MET Start of titration command (Switch on stirrer) The stirrer is switched on after the start. Measure initial measured value The initial measured value is measured. (Start conditions: start volume start meas. value start slope pause) The start volume is added with the start conditions being processed in succession.
4.1 Titrations 4.1.2 Endpoint titrations (SET) Under Start conditions the parameters for the start volume of titrant and for the measurement of the initial measured value are edited: • • • Pause 1 (d): Waiting time, e. g. for electrode equilibration, before a start volume is added. Start volume (d): Volume which is added before the start of the titration. Under Dosing rate (d) you can enter the rate at which the start volume is added.
4 Parameters Parameters for the predefined titration rates for SET SET Titration rate slow optimal fast Control range (Dynamics) 5.000 pH 300.0 mV 40.0 μA 2.000 pH 100.0 mV 10.0 μA 0.500 pH 30.0 mV 5.0 μA Max. rate 1.00 mL/min 10.00 mL/min maximum Min. rate 5.00 μL/min 25.00 μL/min 50.00 μL/min Optimizing the control parameters Reagent addition takes place in three phases during the titration: • • • Initial addition: during this phase the dosing rate increases continuously.
4.1 Titrations steep curves flat curves U/mV Control range U/mV EP Control range EP V/mL V/mL Fig. 4.9: Control range size Editing the parameters for the Stop criterion: • • • Stop criterion (d): The titration stops when the endpoint has been reached and the stop criterion has been fulfilled. The titration can be stopped when a particular (volume) drift has been achieved or after a preset time. If no stop criterion has been selected the titration will not be stopped.
4 Parameters The parameters for the titration sequence are edited under Titration parameters: • • • • Titration direction (d): The titration direction is normally determined automatically from the initial measured value and the set endpoint. It is recommended that, whenever possible, a positive or negative alteration of the measured value is entered. If two endpoints have been set then the titration direction will be defined automatically. In this case the setting will be ignored.
4.1 Titrations terval between the end of conditioning and the end of the determination. If the drift is known for a longer period of time then this can be calculated for the EP-volume by manual drift correction. The result always indicates whether it has been drift-corrected or not. • Drift value (d): Volume drift for manual drift correction • Measured value display: The volume drift can be shown continuously during conditioning. Editing the conditioning options: • Cond.
4 Parameters Titration sequence for SET 1st start of titration command Checks whether work is to be carried out with or without conditioning. (Switch on stirrer) The stirrer is switched on after the start. Preconditioning (if activated) 2nd start of titration command The titration cell solution is titrated to the endpoint and kept there continuously. The method sequence itself starts. Measure initial meas- The initial measured value is measured.
4.1 Titrations 4.1.3 Karl Fischer titrations (KFT) Under Start conditions the parameters for the addition of the start volume of titrant and for measuring the initial measured value are edited. These conditions must be fulfilled before a titration can be started. • • • Pause 1 (d): Waiting time, e. g. for electrode equilibration, before the start volume is added. Start volume (d): Volume which is added added before the start of the titration.
4 Parameters Parameters for the predefined titration rates for KFT KFT Titration rate slow optimal fast Control range (Dynamics) 300.0 mV 40.0 μA 100.0 mV 10.0 μA 30.0 mV 5.00 μA Max. rate 1.00 mL/min maximum maximum Min. increment minimum (= cylinder volume/10000) minimum (= cylinder volume/10000) 5.00 μL Editing the parameters for the Stop criterion: • • • • Stop criterion (d): When the endpoint has been reached and the stop criterion has been fulfilled the titration is stopped.
4.1 Titrations • • when the EP has already been reached). The entry of an extraction time is advisable for samples which only release their water slowly. Temperature (d): Manually entered titration temperature. If a temperature sensor is connected and the temperature measurement is set to automatic or continuous under Sensor (see Section 4.1.5) then the temperature will be measured continuously. Time interval MP (d): Time interval for entering a measuring point in the list of measuring points.
4 Parameters • • adapted to the size of the titration cell in order to prevent any overflow. Cond. stop time: If conditioning takes longer than the time entered here then the process will be stopped. Start reconditioning only at end of method: If this option is switched on then reconditioning will only start when all method commands have been processed. Otherwise reconditioning would start immediately after the titration command.
4.1 Titrations 4.1.4 STAT titrations (STAT) Under Start conditions the parameters for the start volume of titrant and for the measurement of the initial measured value are edited: • • • Pause 1: Waiting time, e. g. for electrode equilibration, before a start volume is added. Start volume: Volume which is added before the start of the titration. Under Dosing rate you can enter the rate at which the start volume is added.
4 Parameters selected minimum rate, the longer it takes until the control point is reached for the first time. The following rule of thumb should be considered in order to obtain as constant a dosing at the control point as possible: Min. rate in μL/min = Expected rate of reaction in μL/min 10 Parameters for the predefined titration rates for STAT STAT Rate of reaction 50 μL/min 100 μL/min 500 μL/min Control range (Dynamics) 1.000 pH 60.0 mV 1.000 pH 60.0 mV 1.000 pH 60.0 mV Max. rate 0.
4.1 Titrations Dosing within the control range: Within the control range the dosing rate is mainly characterized by the minimum rate. The parameters for the titration sequence are edited under Titration parameters: • • • • • • Titration direction: The titration direction is normally determined automatically from the initial measured value and the set control point. It is recommended that, whenever possible, a positive or negative alteration of the measured value is entered.
4 Parameters • Filling rate: Rate at which the dosing cylinder is refilled after the titration. The maximum filling rate depends on the cylinder volume of the exchange or dosing unit used (see Section 3.8.6). Under Monitoring the parameters for monitoring the measured value, the dosing rate (an average rate) as well as the temperature are defined. Remote signals or RS commands can be assigned to the monitored quantities. This can be used, for example, to switch a thermostat on/off if necessary.
4.1 Titrations Measured quantity Stop Upper limit Lower limit Time Fig. 4.11: Action "Exit method" or "Skip command" When selecting Hold, the addition of the reagent is interrupted until the method sequence is continued manually with [Continue]. If the monitored quantity is still outside the limits (including hysteresis), it is not possible to continue the method sequence. Measured quantity Hold [Continue] Upper limit Lower limit Time Fig. 4.
4 Parameters Measured quantity Wait Upper hysteresis Lower hysteresis Upper limit Lower limit Time Fig. 4.13: Action "Wait" Note! If the lower limit is infringed while monitoring the dosing rate, the actions Hold and Wait do not make sense because the average dosing rate becomes smaller and smaller during the waiting time. The valid range can never be reached again. Under Communication a monitored quantity can be assigned to a remote output signal or to an RS-232 command.
4.1 Titrations The parameters for Control device, Sensor, Dosing device and Stirrer are described in the following Section. Titration sequence for STAT Start of titration command (Switch on stirrer) The stirrer is switched on after the start. Measure initial meas- The initial measured value is measured. ured value (Start conditions: Pause 1 Start volume Pause 2) Pause interval 1 is allowed to elapse. The start volume is added. No measuring points are entered in the list of measuring points.
4 Parameters 4.1.5 Control device, sensor, dosing device and stirrer Under Control device you can select the Titrando or the Robotic Titrosampler with which the titration (or measurement or calibration) is to be carried out. This button will only appear when several control devices that are able to execute the corresponding command have been configured under System/Device manager (see Section 3.10). The instrument names are always shown in the selection list.
4.1 Titrations At the start of the titration the validity of the titer and the expiry date of the selected titrant will be checked as well as the GLP test interval for the exchange or dosing unit. The titer (Variable TITER) and the concentration (Variable CONC) are also available for calculation (CALC command, see Section 4.5.1). STAT, ADD, DOS only: A second dosing device can be defined under Tandem dosing in order to enable continuous dosing.
4 Parameters Cylinder volume Max. dosing rate Exchange unit 1 mL Max. flow rate Dosing unit Exchange unit Dosing unit --- approx. 130 mL/h --- --- approx. 300 mL/h 2.25 mL/min 2 mL --- 5.00 mL/min 5 mL 11.25 mL/min 12.50 mL/min approx. 670 mL/h approx. 750 mL/h 10 mL 22.50 mL/min 25.00 mL/min approx. 1.3 L/h approx. 1.5 L/h 20 mL 45.00 mL/min 50.00 mL/min approx. 2.7 L/h approx. 3.0 L/h 50 mL 112.50 mL/min 124.50 mL/min approx. 6.7 L/h approx. 7.
4.1 Titrations 4.1.6 Direct parameters Direct parameters can be defined for all titration commands; these are then shown in a table when the parameter dialog is opened and can be edited directly (see Section 3.16.5). Direct access ("Quick Access") to the edit dialog for selected method parameters simplifies the editing of parameters which need frequent alteration. You can define the parameters to be shown in the list of direct parameters under Direct parameters.
4 Parameters 4.2 Measurements (MEAS) The following measuring modes can be selected: • • • • • • • pH (potentiometric pH measurement) U (potentiometric voltage measurement) T (temperature measurement) Ipol (voltametric measurement with adjustable polarization current) Upol (amperometric measurement with adjustable polarization voltage) Conc (concentration measurement) Cond (conductivity measurement, see Section 4.3). The parameters for the measurement sequence are edited under Measuring parameters.
4.2 Measurements (MEAS) Note! The algorithm is only valid for direct measurements (MEAS Conc) if the following conditions are fulfilled: - The sample preparation must be identical for the standards and the sample i.e. if aqueous standards have been used for the calibration of the sensor the sample has to be prepared in aqueous agent as well. - The ratio sample volume / volume auxiliary solution must be identical with the ratio standard volume / volume auxiliary solution when calibrating the sensor.
4 Parameters • Pause before meas. (d): If stirring is carried out before the measurement, a pause interval can be entered here. No stirring or measuring occurs during this time. The parameters for the dosing device are defined under Dosing device. • • • • Dosing device: Selects the dosing device to be used for the standard addition. All the dosing device connections (MSB) are always shown. Standard: Standard to be used for the dosing.
4.3 Measurements (MEAS Cond) 4.3 Measurements (MEAS Cond) The parameters for the measurement sequence are edited under Measuring parameters. • Signal drift (d): Drift, i.e. the alteration in the measured value per minute that has to be reached for measured value acceptance. off means that the measured value acceptance takes place when the maximum waiting time has elapsed. This may be advisable if the electrode has a very slow response.
4 Parameters 4.4 Evaluation A list of measuring points can have various additional evaluations applied to it. The evaluation (EVAL command) always refers to the last titration or measurement in the method sequence.
4.4 Evaluation mand then it will be shown in red in the list of commands, as the reference is missing. You can also insert EVAL commands in the method sequence at a later date and trigger the re-evaluation under Results with [Recalculate]. The data for each evaluation can be shown under Results/More determination data/View data and can be calculated in CALC commands. 4.4.1 Evaluation of fixed endpoints (EVAL FIX EP) Fixed endpoints can be determined for all titrations and measurements (except MEAS Conc).
4 Parameters 4.4.2 Evaluation of pK value and half neutralization potential (EVAL pK/HNP) The pK value can be determined for pH titrations (DET and MET) and the half neutralization potential can be determined for U titrations. The activities of conjugated acid-base pairs are linked by the following equation (Henderson-Hasselbalch equation): pH = pKa + log (aB/aA) If the activities of the acid and the conjugated base are equal (aA = aB), then pH=pKa.
4.4 Evaluation 4.4.3 Evaluation of minimum and maximum (EVAL MIN/MAX) For the minimum or maximum measured value the associated volume, time and temperature are interpolated from the list of measuring points. The evaluation begins as soon as the slope of the curve exceeds a particular threshold value. • • Evaluation: In an EVAL MIN/MAX command either the minimum or the maximum can be evaluated. If you require both values then you must define a second EVAL MIN/MAX command in the method sequence.
4 Parameters 4.4.4 Evaluation of break points (EVAL BREAK) A break point evaluation is used to determine sharp change of direction in the titration curve. This evaluation is primarily used for photometric and conductivity titrations. The method is based on the search for extremes in the second derivative of the curve. • • • • EP criterion: Measure for the minimum sharpness of the break. The smaller the EP criterion set, the more break points will be found.
4.4 Evaluation Measured value 2nd Derivative Break point Volume or Time Fig. 4.17: Evaluating a breakpoint 4.4.5 Rate evaluation (EVAL RATE) The rate evaluation produces the average dosing rate in a defined range (so-called window). The average dosing rate is determined by linear regression using at least three measuring points. If dosing is carried out with one dosing device only and more than one cylinder volume is dosed then the average dosing rate will be reduced because of the filling time.
4 Parameters If the limit value is between two entries of the measuring point list then the next measuring point outside the window is included in the calculation.
4.5 Calculations 4.5 Calculations In the method sequence result calculations can be defined with the CALC command. A method can contain a maximum of nine CALC commands each with nine result calculations. The CALC commands also contain instructions for statistical calculations, titer assignments, storing common variables and storing results in the result silo. Limits can also be defined for the results.
4 Parameters The result template chosen in the selection list is loaded with [Load template] and a note concerning the template is shown. With [Custom templates] you can open the list of your own result templates (see Section 3.14.3, Section 4.5.4 and Section 4.5.5). Use [Empty result] to open the edit dialog directly. • • • • Result name: The standard result name corresponds to the result variable. The result name is the text which will be shown in the result display and in the report.
4.5 Calculations • • • • • • always be shown as the default value. If no mean value is to be calculated for a result this variable should be set to off. The mean value for the result can be accessed via the statistics variable for further calculations. Save result as titer: The result can be saved as a titer. The titer is assigned to the titrant defined in the last titration command before the calculation.
4 Parameters Open the dialog Edit result/Result limits and activate the Monitoring result limits checkbox. Enter an Upper limit and a Lower limit for the result. If a result is invalid then it will be treated as if the limits had been infringed. The following actions are available if the result limits are infringed: • • • Display message: The run is halted and a message is shown. You can choose whether you want to terminate the run or continue with it.
4.5 Calculations 4.5.2 CALC LIVE command The CALC LIVE command must be inserted directly before the corresponding titration or measuring command. The CALC LIVE command is identical with the CALC command except for the following differences: • • • • • The number of the variables which can be calculated is limited. No result options are available. The result cannot be monitored. The result variable cannot be altered. The live result is displayed only during a running titration or measurement.
4 Parameters 4.5.3 The formula editor The formula editor is used to enter the formulas for the result calculations. The formula editor has an automatic syntax check, which is triggered when the formula is accepted. The priority rules which are normally valid apply to the calculation operations. The result variable is shown in front of the input field. Buttons are available for entering numbers, mathematical operators and variables. The backspace key [⌫] deletes the character in front of the cursor.
4.5 Calculations The selected variable is entered in the formula with [Insert] or [Back]. With [Cancel] you can exit the list without accepting a variable. The individual variables are described in Section 4.5.7. The character # stands for a running number (usually from 1 to 9 or 10); this must be entered manually. If you want to calculate EP1, for example, then EP is inserted in the formula and you must enter the 1 in the formula editor.
4 Parameters If the method contains more than one CALC command then the command identification will be given before the variable (e. g. 1C.R1 for the result variable R1 to be calculated in the first CALC command). Result variables which are to be calculated in the CALC command which is currently being edited are given without any command identification. You can open the list of common variables with [Common Variables]. In the formula editor you can use [Math.
4.5 Calculations If invalid variables (e. g. missing endpoints) could occur in a result calculation then these can be replaced with a valid value (replacement value) by using the test function TST. In this way invalid results can be avoided. Syntax: TST (variable to be tested, replacement value) 4.5.4 Creating custom result templates Under System/Templates/Custom result templates you can create templates for result calculations (see Section 3.14.3).
4 Parameters Select a result template from the list and load it with [Load template]. The F-variables used in the result template are automatically requested when the template is loaded if the display of the note is closed by pressing [Next]. The only input fields which are active are those for the variables used in the result template. The entered values will be inserted automatically in the calculation formula in place of the variables.
4.5 Calculations 4.5.6 Conversion table of the calculating formula for KF titrations water content = [volume(KF - reagent) − blank ]⋅ titer ⋅ factor sample size ⋅ divisor Result unit Sample size in... Factor Divisor % g 0.1 1 % mg 100 1 % mL 0.
4 Parameters ables with the necessary command identifications are shown in the list of variables. Attention! If you subsequently enter commands in the list of commands, then the command identifications of the variables in the calculations will not be adapted automatically. Variable Description Method command C00 Sample weight all CI1 CI2 Sample identification 1 and sample identification 2 The sample identifications can be used in calculations if numerical values are entered.
4.5 Calculations 250 Variable Description Method command MIT Initial temperature (temperature before start conditions are processed) DET, MET, SET, KFT, STAT, MEAS, DOS MSA Start volume which is added according to the start volume given in the start conditions. DET, MET MSP Start volume which is added according to the start measured value given in the start conditions. DET, MET MSS Start volume which is added according to the start slope given in the start conditions.
4 Parameters Sensor Evaluation fixed endpoints Evaluation pK value / half neutralization potential Evaluation minimum Evaluation maximum Evaluation break point PC Control / Touch Control Variable Description Method command MMP Number of measuring points in the list of measuring points DET, MET, SET, KFT, STAT, MEAS, DOS MTS Stop type (termination of the titration, measurement or calibration), format: text DET, MET, SET, KFT, STAT, MEAS, DOS, CAL MEN Electrode zero point pH(0) or E(0) DET,
4.
4 Parameters 4.5.8 Result variables as parameters In many numerical entries for method parameters you can also enter a result which has previously been calculated (e. g. R1) instead of a number. The result must have been calculated in a previous CALC command in the method sequence. Please note that the result must be within the input limits for the parameter, as otherwise the determination run will be halted when the parameter is accessed.
4.6 Reports 4.6 Reports In the REPORT command you can define a maximum of ten reports which can be printed out in the method sequence. The reports which are defined in a report command are printed out in the sequence in which they are entered in the list. You can insert a report in the list in front of the selected line with [Insert]. You can use [Method reports] to open the list of reports for the current method. [System reports] opens the list of reports for systemspecific data.
4 Parameters In the report header the type, serial number and program version of the software (Touch Control or PC Control), the device name which you can enter in the device manager of Touch Control or PC Control and the printout date with time zone can be printed out. You can also define your own report header under System/Templates/Report header; this will be printed out before the standard report header (see Section 3.14.7).
4.6 Reports Report Parameter List of measuring points - Selection of the titration or measurement (mode) for which the list of measuring points is to be printed out. Calculations - Determination properties (on/off) - The variables can be printed out as shown or with the full accuracy of the floating point number ("double precision" to Standard IEEE 754). Devices used Determination properties (on/off). Variables All determination date; depends on command.
4 Parameters 4.7 Calibrating pH electrodes (CAL pH) and ISE (CAL Conc) For pH measurements, titrations to a preset endpoint (SET pH) and the determination of pK values and fixed endpoints the calibration of the pH electrode (command CAL pH) is essential; it is also recommended for all other pH titrations. As least two buffers should be used for the calibration; these should cover the expected measuring range.
4.7 Calibrating pH electrodes (CAL pH) and ISE (CAL Conc) For automatic calibrations with the USB Sample Processor the parameter USB must be selected. The CAL command must be called up in a subsequence (see Section 4.12.6) with the subsequence option "Cycles = Calibration". In order to change the calibration solution a MOVE command (see Section 4.12.1) must be inserted before the CAL command with the target "Calibration pos.". The 1st calibration position must be defined in the rack table (see Section 3.
4 Parameters • • Unit Conc. (d): Select the concentration unit of the standard. The concentration unit for concentration measurements always depends on the unit entered for the concentration of the standard. Conc. standard 1 to Conc. standard 5 (d): Enter the concentration for 1 to 5 concentration standards. off means that the standard and all those following will not be used. During the sequence a message will appear the corresponding number of times to indicate the next standard to be used.
4.7 Calibrating pH electrodes (CAL pH) and ISE (CAL Conc) (Switch on stirrer) The stirrer will be switched on if Stir solution during measurement is activated. Measure buffer 1 The potential of buffer 1 is measured. (Switch off stirrer) The stirrer will be switched off if the buffer has been recognized and if Stir solution during measurement is activated. Message showing which buffer has been recognized. A message will be shown with instructions for the next buffer.
4 Parameters At the end of the determination sequence the calibration data is shown on the result page.
4.7 Calibrating pH electrodes (CAL pH) and ISE (CAL Conc) Concentration calibration with up to 5 standards Immerse electrode in first standard Start the calibration command Measure or enter If a temperature sensor is connected then the the calibration tem- temperature will be measured. Otherwise a query perature will appear and the temperature must be entered manually. Repeat for each standard Message A message appears with instructions for the first standard. Start the measurement with [OK].
4 Parameters 4.8 Calibrating conductivity measuring cells (CAL Cond) The cell constant of a conductivity measuring cell can be determined with the CAL Cond command. Under Calibration parameters you can edit the parameters for the calibration sequence. • • • • Signal drift (d): Drift, i.e. the alteration in the measured value per minute that has to be reached for measured value acceptance. off means that the measured value acceptance takes place when the maximum waiting time has elapsed.
4.8 Calibrating conductivity measuring cells (CAL Cond) The parameters for Control device, Sensor and Stirrer are described in Section 4.1.5. Note! Make sure that the sensor to be calibrated has been selected under Edit command/Sensor. This is the only way to ensure that the calibration data for this sensor is stored in the correct place under System/Sensors. The choice of the Direct parameters is described in Section 4.1.6.
4 Parameters 4.9 Electrode test for pH electrodes (ELT) For pH electrodes you can carry out an automatic electrode test which allows the quality of the electrode used to be evaluated. As the result you will obtain various information about the characteristic measuring properties of your pH electrode (slope, response time etc.). The concluding evaluation of the electrode is carried out by checking the results obtained against preset limit values.
4.9 Electrode test for pH electrodes (ELT) Under Electrode test parameters you can edit the parameters for the electrode test sequence. • • • • Buffer type: Selects a predefined buffer series for the calibration. The following buffer series are available: Metrohm, NIST, DIN, Fluka Basel, Mettler, Merck Titrisol, Radiometer, Merck CertiPUR, Baker, Hamilton, Precisa. The temperature tables for the buffer series can be found in Section 6.4.
4 Parameters Note! Make sure that the sensor to be calibrated has been selected under Edit command/Sensor. This is the only way to ensure that the calibration data for this sensor is stored in the correct place under System/Sensors. Sequence of the electrode test Note! In order to obtain realistic response times the electrode should be immersed in each buffer at about the same time as the measurement is started and it should be positioned directly above the stirrer which has already been switched on.
4.9 Electrode test for pH electrodes (ELT) Limit values of the three electrode types Rating Excellent electrode Good electrode Usable electrode Streaming potential 2.5 mV 3.0 mV 4.0 mV Drift 2.0 mV/s 2.5 mV/s 3.0 mV/s Slope min. 96.5 % 96.0 % 95.0 % Slope max. 101.0 % 102.0 % 103.0 % Response time 45 s 50 s 60 s Electrode type "Standard" Lower limit Uoff –15 mV Upper limit Uoff 15 mV Electrode type "Gel" Streaming potential 3.0 mV 3.5 mV 4.5 mV Drift 2.5 mV/s 3.0 mV/s 4.
4 Parameters Possible errors of the electrode test Test criterion Message Measure pH 9: The drift in stirred solution is > 1 mV. General problem - Connect electrode. - Replace defective electrode cable. - Clean diaphragm (see electrode leaflet). - Replace electrode. pH 9: –10 mV < U(unstirred) < 10 mV and the sum of drift values after 1, 2, 3 und 4 min is < 12 mV/min. Short circuit Replace electrode. A response time does not meet the limit value for the rating "Usable electrode".
4.10 Dosing and liquid handling 4.10 Dosing and liquid handling With the dosing commands you can add a fixed volume in the method sequence; exchange or dosing units can also be prepared and emptied automatically. Complex dosing tasks can be carried out comfortably with the liquid handling commands. 4.10.1 Dosing (ADD) The ADD command is used to add a preset volume of a solution. • • • Volume (d): Volume to be added. Dosing rate (d): Rate at which the volume is to be added.
4 Parameters • • • • Function: Selects the possible working steps. With Dosing the given volume is added. Automatic filling takes place neither before nor after the command. Fill the cylinder can take place from a freely selectable port. The valve disk then remains at the selected port. With Aspirate liquid is aspirated via the given port. As with Dosing, the cylinder is not automatically filled either before or after the command.
4.10 Dosing and liquid handling 4.10.3 Preparing (PREP) and emptying (EMPTY) Preparation is used to rinse the cylinder and the tubing. Empty is used to empty the cylinder and the tubing. The empty command is only available for Dosino-type dosing devices. • • • • • Control device: Selects the control device (Titrando, USB Sample Processor etc.) to which the dosing device is connected and which is to be prepared or emptied.
4 Parameters 4.10.4 Monitored dosing (DOS) A predefined volume of a solution is dosed with the DOS command. The measured value and the temperature are monitored simultaneously. • Dosing criterion: Two parameters from the following can be defined: Volume, Dosing rate and Dosing time. The third parameter is calculated according to the following formula: Volume = Dosing time ⋅ Dosing rate If continuous dosing is required, a tandem dosing setup (see Section 4.1.5) can be used i.e.
4.10 Dosing and liquid handling Single dosing V/mL Tandem dosing V/mL Filling time t1 t2 t/s t/s t1 + t2 Fig. 4.19: Definition of volume and dosing time If the dosing rate resulting from the settings cannot be achieved dosing is carried out at maximum rate. The following formula can be used to estimate whether the maximum dosing rate is necessary or not: Dosing rate = Desired flow rate in mL/min ⋅ 2.22 Note! This formula applies only for using a single dosing device.
4 Parameters Flow rate of a single dosing device The cylinder volume and the filling time of the exchange or dosing unit must be taken into account for the calculation of the effective flow rate. Max. flow rates for different cylinder volumes: Cylinder volume Max. flow rate Exchange unit Dosing unit 1 mL approx. 80 mL/h --- 2 mL --- approx. 170 mL/h 5 mL approx. 400 mL/h approx. 430 mL/h 10 mL approx. 800 mL/h approx. 860 mL/h 20 mL approx. 1.6 L/h approx. 1.7 L/h 50 mL approx.
4.10 Dosing and liquid handling Example: 1 L reagent has to be dosed within 1 hour with a 50 mL exchange unit. What is the dosing rate? Total duration = 60 min Volume = 1000 mL Filling time = 24 s (at max. filling rate) Cylinder volume = 50 mL Number of refills = Volume 1000 = = 20 Cylinder volume 50 If the division delivers an integer number, the last filling is no longer a refilling and must be deducted. In our example, 19 refills are necessary. There is no dosing during this time i.e.
4 Parameters • • temperature will be measured continuously. The value is used for temperature compensation in pH measurements. Time interval MP: Time interval for entering a measuring point in the list of measuring points. The list of measuring points can contain max. 1000 measuring points. Pause: Waiting time, e. g. for electrode equilibration, after the start of the method.
4.11 Communication 4.11 Communication With the communication commands SCAN and CTRL you can scan and set remote lines at a connected remote box. The connection of the remote box is described in the Installation Instructions for the Titrando. The pin occupancy of the remote connection and the functions of the individual remote lines are described in Section 6.2. The commands SCAN RS and CONTROL RS are for the communication with peripheral devices which are connected via a serial RS-232 interface. 4.11.
4 Parameters wish to use a pulse with a pulse length other than 200 ms then you must define a corresponding template. We recommend that non-relevant output lines are also masked with an asterisk (*) in order that the condition of these lines is not altered. The templates are described in Section 3.14.5. 4.11.3 Receive data (SCAN RS) Definition of the parameters for receiving data via a serial RS-232 interface.
4.12 Automation 4.12 Automation The automation commands, with the exception of the subsequence, are only active when a USB Sample Processor has been configured in the Device manager (see Section 3.10). A connected USB Sample Processor is controlled with these commands in the method sequence. 4.12.1 Move (MOVE) The MOVE command is used to move to a rack position or an external position. • • 280 Tower: The required tower can be selected here.
4 Parameters • • The sample rack can be rotated by a certain increment independently from a rack position with the function +/- rotate. The robotic arm can also be swung by a certain increment independently from the position with +/- swing. The values of the rotation and swing increment are defined in the device properties of the tower and of the Swing Head respectively (see Section 3.10.5).
4.12 Automation 4.12.4 Rack reset (RACK) With the command Rack reset the rack, lift and robotic arm are reset, the rack code is read off and the corresponding rack data is transferred to the USB Sample Processor. At the same time the sample variable is reset to one. • Check rack: The rack which is put on can be checked at the start of the method. In this way you can ensure that the method can only be carried out with this rack.
4 Parameters The list with templates for subsequences is displayed under Edit Subsequence/Load: Open the list with your [Own subsequences]. You have now the possibility to load or to delete your own subsequence. Under [Subsequence options] parameters are set that refer to the whole subsequence: • PC Control / Touch Control Subsequence type: The type of subsequence is entered here. A Sample sequence is carried out each time that a method is run.
4.12 Automation • The Conditioning sequence will be carried out just before the conditioning. It gives you the opportunity, for example, to start a connected Polytron® high-frequency homogenizer and to set its stirring rate before the start of the conditioning. Use the CONTROL RS command for this. Cycles: A subsequence is repeated in accordance with the number of runs. "Calibration" is required if automatic calibration is to be carried out with a USB Sample Processor.
4 Parameters 4.13 Various commands Various commands are brought together in the command group Miscellaneous: switching the stirrer on/off, defining a waiting period or stopping the run, requesting sample data or common variables, acoustic signal, signing the determination and stopping the method sequence. 4.13.1 Stirring (STIR) The STIR command is used to switch a connected stirrer on or off. • • • • Control device: Selects the control device (Titrando, USB Sample Processor etc.
4.13 Various commands 4.13.3 Requesting sample data and common variables (REQUEST) With the REQUEST command you can request sample data (sample identification 1, sample identification 2 and sample size) or a common variable during the method sequence. You can choose whether the run is to be stopped or whether it should continue in the background. • • • • • Sample identification: Select the sample identification(s) to be requested in the sequence.
5 Troubleshooting – Maintenance 5 Troubleshooting – Maintenance This section contains troubleshooting information and a description of the diagnosis functions integrated in Touch Control and PC Control. For Touch Control a description is given of how to change the batteries and carry out a "RAM initialization". 5.1 Troubleshooting This section describes several problems that could occur when operating the system together with possible causes and their remedies. 5.1.
5.1 Troubleshooting 5.1.3 288 Results, calculations and statistics Problem Possible cause Remedy No statistics are carried out for a result. The Statistics function has not been activated in the method under Sequence/ Method options. Activate the statistics function under Sequence/Method options (see Section 3.16.4). No Variable for mean has been selected in the method for the result calculation.
5 Troubleshooting – Maintenance 5.1.4 SET titrations Problem Possible cause Remedy Dosing at the end takes too long and the increments are too small. Max. rate too low. Increase the min. rate under Control parameters/User-def. parameters. Unfavorable Stop criterion. Try increasing the Stop drift or select a shorter Delay time. The titration is not controlled properly, i.e. individual increments are not added at the end. - Select the Titration rate slow under Control parameters.
5.1 Troubleshooting 5.1.5 KF titrations Problem Possible cause Remedy Dosing at the end takes too long and the increments are too small or the conditioning takes very long, high drift. Inappropriate solvent, pH value suboptimal (side reactions) Change the solvent with problematic samples e. g. 2methoxyethanol for ketones or aldehydes or a mixture of methanol/glacial acetic acid for amines, see technical literature.
5 Troubleshooting – Maintenance Problem Possible cause Remedy The drift increases with every titration. Does your sample evolve water extremely sluggishly? Adjust the method, add solubilizer, work at increased temperature (poss. use KF oven), see technical literature. Are acids esterified in your sample? Change the solution more frequently and increase the buffer capacity of the solvent. Does your sample contain ketones or aldehydes? Use special reagents suitable for ketones and aldehydes.
5.1 Troubleshooting Problem Time for reaching the control point is too long. 5.1.7 Remedy Cylinder volume of exchange/dosing unit is too large. Use an exchange/dosing unit with a smaller cylinder volume (smaller volume increment per pulse). Electrode responds to slowly. Replace the electrode. Unfavorable control parameters. - Select a smaller Dynamics under User-defined parameters. - Increase the Min. rate under User-defined parameters. - Increase the Max. rate under User-defined parameters.
5 Troubleshooting – Maintenance Problem Possible cause Remedy Touch Control: The error message "No printer" is displayed when printing manually or when starting a method with a REPORT command. The USB printer has been switched off while the Touch Control was running. Switch on the printer again and switch off and back on the Touch Control. 5.1.9 Manual Operation Problem Possible cause Remedy The [Manual] fixed key is inactive. The [Manual] fixed key is deactivated.
5.1 Troubleshooting 5.1.11 File manager Problem Possible cause Remedy Files, e. g. methods, which have been saved on a data card by a PC, cannot be read by Touch Control. Windows Explorer has been used for copying and the correct folder structure has not been maintained (see Section 3.11). Use PC Control to copy the files. 5.1.12 Miscellaneous 294 Problem Possible cause Remedy Touch Control cannot be switched on. Touch Control is connected to an MSB socket of the Titrando.
5 Troubleshooting – Maintenance 5.2 Diagnosis You can carry out selective tests on the Titrando system or trigger special functions. Select Diagnosis in the System menu: The diagnosis functions are written in English and are all available for the Touch Control. With PC Control the selection is limited to those functions marked with an *. 5.2.1 LCD test With the LCD test you can check the function of the Touch Control display. Press [LCD test]. The whole screen appears in white.
5.2 Diagnosis 5.2.3 Formatting a memory card (Format card) Select [Format card] in order to format a PCMCIA or CompactFlash memory card inserted in the Touch Control. Select the memory card to be formatted (Card 1 / Card 2) and the formatting mode. With normal the memory card will be completely cleared; with quick only the "main folder" of the card will be overwritten with zero so that the whole capacity is again available. Start formatting with [Format] and answer the safety query with [Yes].
5 Troubleshooting – Maintenance Last square to be touched appears in green. Next square to be touched appears in red. Crosshair shows last recognized contact point. Variation of the recognized contact point from the center of the last square touched. You can use [Back] to switch back again step by step. When you have checked all the display areas a list of fixed keys appears; you should touch them in any sequence. If they function correctly the request will always change to an appropriate message (e. g.
5.2 Diagnosis Program version Information about the existing program version is given under System/Device manager. Select the corresponding device and press [Edit]. Data source If PC Control is used then the firmware of the control device should be available on one of the data carriers of the computer. This could be a hard disk, CD-ROM or a PCMCIA or CompactFlash card connected by a card reader. The Touch Control requires the program files on a memory card in Card slot 1 (Card 1).
5 Troubleshooting – Maintenance Loading a new dialog language (Touch Control only) Note! Only one additional language can be installed besides English as the standard language. If there is already a second language installed, it will be overwritten. In the System/Diagnosis/Software update menu select Touch Control under Device. In the selection list Update type, select the item Second language and confirm with [Continue]. Under Binary file, open the list with the program files on the memory card.
5.2 Diagnosis PC Control: When the update has been completed you must shut down the PC Control software. This is done by pressing [Back] or [Home] and confirming the following message with the request for a restart with [OK]. The PC Control program ends automatically. Restart PC Control. Touch Control: When the update has been finished you must switch off the Touch Control, wait a few seconds, and then switch it on again.
5 Troubleshooting – Maintenance 5.2.8 822 Curve Simulator The 822 Curve Simulator can be used as a diagnosis tool for checking the recording of the titration curves and their evaluation. Titration methods can be carried out and simulated measuring curves recorded without the actual presence of a measuring solution. Details about the connection and operation of this instrument are given in the appropriate Instructions for Use.
5.2 Diagnosis 5.2.9 Remove PCMCIA card 1/2 As long as the Touch Control is not accessing the data on the inserted memory card for loading or storing you can remove and insert the memory card without any problems with the Touch Control switched on. This option offers additional data protection as it ensures that the data to be stored is completely written onto the card before the power supply to the card is switched off.
5 Troubleshooting – Maintenance 5.3 5.3.1 Maintenance Changing the batteries (Touch Control only) The Touch Control indicates that its batteries need changing with the message "Battery low". Please note that the current date and time will be reset to 1.1.2000 and 00:00:00 respectively. Proceed as follows: Switch off the Touch Control. Remove the three fastening screws of the protective cover on the base of the housing: Fig. 5.
5.3 Maintenance 5.3.2 RAM initialization (RAM Init, Touch Control only) In very rare cases excessive interference could affect the functions of the processor and cause a program crash. In this case the RAM sector must be initialized. RAM initialization is also the only way of making the system accessible again if it is impossible for a user to log in because, for example, even the Administrator has forgotten the password or no Administrator has been defined (see Section 3.7.5).
6 Appendix 6 Appendix In this section you will find the most important technical data for the Touch Control, a list of standard accessories and optional accessories for the Touch Control and PC Control software as well as the warranty and declarations of conformity. 6.1 Technical data Provided that nothing to the contrary is mentioned, the published values represent typical technical data for the Touch Control. 6.1.1 6.1.
6.1 Technical data 6.1.5 6.1.6 Electromagnetic compatibility (EMC) Emission Standards fulfilled: - EN/IEC 61326-1 - EN/IEC 61000-6-3 - EN 55022 / CISPR 22 Immunity Standards fulfilled: - EN/IEC 61326-1 - EN/IEC 61000-6-2 - EN/IEC 61000-4-2 - EN/IEC 61000-4-3 Ambient temperature Nominal working range Storage Transport 6.1.7 306 +5 °C...+40 °C (at max. 85% rel. humidity) –20 °C...+60 °C –40 °C...
6 Appendix 6.2 Remote box The 6.2148.010 Remote box allows devices to be controlled which cannot be connected directly to the MSB interface of the Titrando, e. g. Level Control 849. The connection of the Remote box is described in the Installation Instructions for the Titrando. Fig. 6.1: View of the connections of the optional 6.2148.010 Remote box 6.2.
6.2 Remote box 6.2.2 Functions of the individual remote lines Name Input 0 Function Pin. 21 START On activation the current method is started. tpulse > 100 ms Input 1 9 STOP On activation the current determination is halted (Stop). tpulse > 100 ms Input 3 10 CANCEL On activation the current command in the determination run will be halted. tpulse > 100 ms Input 4 23 - Not occupied, can be used for scanning the Sample Processor (sample in work position). Input 5 11 - Not occupied.
6 Appendix 6.3 RS-232/USB Box If Touch Control is used then the 6.2148.020 RS-232/USB Box allows devices with a serial RS-232 interface to be directly connected to the Titrando. Such a device could be a balance or computer for data transmission. The connection of devices via the RS-232/USB Box is described in the Installation Instructions for the Titrando. Fig. 6.3: View of the connections of the optional RS-232/USB Box 6.3.
6.3 RS-232/USB Box 6.3.2 RS-232 pin occupancy RS-232 connection: D-sub 9-pole, male, full Fig. 6.
6 Appendix 6.4 Stored buffer series for CAL pH For automatic buffer recognition during pH calibration the temperaturedependent pH values of several common pH buffers are stored in the system. Apart from the Metrohm buffer solutions other reference and technical buffers are also included in the tables. The following tables provide an overview of the stored pH(T) series: The pH values printed in bold are the values at the reference temperature of the particular buffer set.
6.4 Stored buffer series for CAL pH DIN (according to DIN standard 19267, 1978) Temp. (°C) DIN1 DIN3 DIN4 DIN7 DIN9 DIN12 pH 1 pH 3 pH 4 pH 7 pH 9 pH 12 0 1.08 - 4.67 6.89 9.48 - 1) 1) 5 1.08 - 4.66 1.09 3.10 4.66 6.84 9.37 13.37 15 1.091) 3.081) 4.651) 6.821) 9.321) 13.151) 20 1.09 3.07 4.65 6.80 9.27 12.96 25 1.09 3.06 4.65 6.79 9.23 12.75 30 1.10 3.05 4.65 6.78 9.18 12.61 35 1.10 40 1.10 1) 45 1.10 50 1.11 1) 55 1.11 60 1.
6 Appendix Mettler Toledo Temp. (°C) Beckman MT2 MT4 MT7 MT9 MT11 Bec4 Bec7 Bec10 pH 2 pH 4 pH 7 pH 9 pH 11 pH 4 pH 7 pH 10 1) 1) 1) 1) 1) 4.00 7.12 10.32 0 2.03 4.01 7.12 9.52 11.90 5 2.02 4.01 7.09 9.45 11.72 4.00 7.09 10.25 10 2.01 4.00 7.06 9.38 11.54 4.00 7.06 10.18 15 2.00 4.00 7.04 9.32 11.36 4.00 7.04 10.12 20 2.00 4.00 7.02 9.26 11.18 4.00 7.02 10.06 25 2.00 4.01 7.00 9.21 11.00 4.00 7.00 10.01 30 1.99 4.01 6.99 9.
6.4 Stored buffer series for CAL pH Hamilton DURACAL Precisa Temp. (°C) Ham4.01 Ham7.00 Ham9.21 Ham10.01 Pre4 Pre7 Pre9 pH 4.01 pH 7.00 pH 9.21 pH10.01 pH 4.00 pH 7.00 pH 9.00 0 - - - - 3.99 7.11 9.27 5 4.01 7.09 9.45 10.19 3.99 7.08 9.18 10 4.00 7.06 9.38 10.15 3.99 7.06 9.13 15 4.00 7.04 9.32 10.11 3.99 7.04 9.08 20 4.00 7.02 9.26 10.06 3.99 7.02 9.04 25 4.01 7.00 9.21 10.01 4.00 7.00 9.00 30 4.01 6.99 9.16 9.97 4.00 6.99 8.96 35 4.
6 Appendix Merck CertiPUR (25 °C) Temp. (°C) MerC4.01 MerC7.00 MerC9.00 MerC10.00 pH 4.01 pH 7.00 pH 9.00 pH 10.00 0 - - - - 5 4.00 7.09 9.22 10.22 10 4.00 7.06 9.16 10.16 15 4.00 7.04 9.10 10.10 20 4.00 7.02 9.05 10.05 25 4.01 7.00 9.00 10.00 30 4.01 6.98 8.96 9.94 35 4.03 6.98 8.93 9.90 40 4.03 6.97 8.89 9.86 45 4.05 6.97 8.87 9.80 50 4.06 6.97 8.84 9.
6.5 Liquid handling – schematic process 6.5 6.5.1 Liquid handling – schematic process Port definitions of the dosing unit VENT Port 3 Port 1 Port 4 Port 2 Fig. 6.5: Port occupancy of the Dosing unit 6.5.2 VENT – is intended for venting the storage bottle and is normally fitted with an adsorber tube (filled with a drying agent). Port 1 – is side-mounted; its default definition is as dosing port 1.
6 Appendix 6.5.3 Pipetting sequences Principle Measuring out the liquid to be pipetted takes place in the pipetting tubing, which is filled with a carrier liquid (preferably water). In order to avoid carryover or mixing an air bubble (separating bubble) must be inserted between the sample and the carrier liquid. The tubing tip should be drawn out by hand to form a fine point. A Dosino drive is used to transfer the liquids to the tubing. The pipetting tubing is attached to Port 1 of the dosing unit.
6.5 Liquid handling – schematic process The titration cell can then be sucked off, rinsed and prepared with fresh solvent. Pipetting The pipetting procedure takes place in five steps: • • • • • Eject cylinder contents (see above) and form separating bubble Move to sample Aspirate / Measure out sample Move to target Eject sample These five Steps can be combined to a subsequence defined as Sample sequence (see Section 4.9.6).
6 Appendix The titration cell should be filled with solvent before the sample is added so that the sample can be pipetted directly into the liquid (tip immersed). Command sequence: LQH MOVE LIFT change port move to titration cell move to work position Eject sample The sample should be ejected at a reduced dosing rate (< 10 mL/min). The appropriate settings can be made in the liquid handling command under Rate.
6.6 Titration and measuring modes in the Titrando system 6.6 Titration and measuring modes in the Titrando system Device 1) 2) 320 808 809 835 836 841 842 857 855 DET • • • • – – • • MET • • • • – – • • SET • • • • • • 1) • • KFT – – • • • – • – STAT – – • • – • 1) • • MEAS • • • • • • 1) • • MEAS Conc • • • • – – • • CAL • • • • • 2) • 2) • • DOS – – • • – • • • no U(pol), I(pol) no CAL Conc.
6 Appendix 6.7 Import of Titrino methods (PC Control only) With the Titrino method converter you can import Titrino methods into the PC Control software. Use the Metrohm VESUV software to save the methods which are stored in the Titrino. The methods are stored in a .vmb file. In the File menu open the menu item Import Methods... Use [Open method] to open the Vesuv backup file dialog. Select the required .vmb file and open it. The methods are listed under Select methods.
6.7 Import of Titrino methods (PC Control only) The methods are shown in color. The colors have the following meanings: • • • Green: conversion OK. Yellow: 1:1 not possible. The converted method must be checked. Red: conversion not possible. If you click on the method name then all the messages referring to this method will be shown in a new dialog window. The following messages may be produced: Conversion OK (green-marked methods) • • • The method has been converted successfully.
6 Appendix • • • • • • • • • • • The assignment of sample identification 3 (C23) to a common variable is not possible. The assignment of sample identification 3 (C23) to a statistics variable is not possible. A formula contains the sample identification 3 (C23). The variable has been replaced by -0. The method contains the parameter 'activation pulse: first'. This parameter has been ignored. Measuring input 'diff.' has been replaced by measuring input '1'. The relative start volume has been replaced by 0.
6.8 Arithmetic algorithms in the Titrando 6.8 Arithmetic algorithms in the Titrando Some of the algorithms and number formats used in the instrument software are explained subsequently. Number format The standard IEEE 754 (1985) for binary floating-point arithmetic has been implemented in the software as "single precision" (32 Bit). Rounding method Measured values and results are displayed rounded, depending on user settings.
6 Appendix Explanation The statistical calculations in the software have been implemented in such a way that they are as revisable as possible for the user. This is why the individual values used in the statistics are in the rounded presentation form selected by the user. It is not the number of decimal places which is decisive for the accuracy of the calculations, but rather the number of significant digits of the decimal numbers displayed.
6.9 Standard equipment 6.9 Standard equipment Immediately upon receipt of the Touch Control or PC Control software please check that the delivery is complete. Please also consult the lists of accessories in the Installation Instructions for the Titrando, where the Titrando accessories are described. 6.9.1 No. 840 Touch Control Order no. Description 1 1.840.0100 840 Touch Control 1 6.6051.000 CompactFlash card with user methods and 6.2247.000 Adapter 1 A.704.0007 PC Control CD-ROM 1 8.840.
6 Appendix 6.10 Additional devices and optional accessories 6.10.1 Miscellaneous accessories Order no. Description 6.2145.100 USB dongle 6.2162.000 Bluetooth USB adapter for Touch Control 840 6.2051.030 Wall holder for attaching the Touch Control to a wall or support rod (diameter 10 mm). You can also use the wall holder to achieve a steeper display angle on the bench. 6.2834.030 Spare film for 840 Touch Control 3 pieces The films can be exchanged when they become dirty or damaged.
6.10 Additional devices and optional accessories 328 Order no. Description 6.2151.
6 Appendix 6.11 Warranty and conformity 6.11.1 Warranty Metrohm guarantees that the deliveries and services it provides are free from material, design or manufacturing errors. The warranty period is 36 months from the day of delivery; for day and night operation it is 18 months. The warranty remains valid on condition that the service is provided by an authorized Metrohm service organization. Glass breakage is excluded from the warranty for electrodes and other glassware.
6.11 Warranty and conformity 6.11.2 Declaration of Conformity Software Validation CH-9101 Tel. Fax Herisau, Switzerland +41 71 353 85 85 +41 71 353 89 01 www.metrohm.com for the program PC Control 5.0 Description PC software for controlling Metrohm titration and automation instruments. Simple and intuitive user guidance. Creation of methods, carrying out titrations, storage and recalculation of results. Methods and data are compatible with Touch Control.
6 Appendix 6.11.3 Declaration of Conformity This is to certify the conformity to the standard specifications for electrical appliances and accessories, as well as to the standard specifications for security and to system validation issued by the manufacturing company. Name of commodity 840 Touch Control Description CH-9101 Herisau/Switzerland E-Mail info@metrohm.com www.metrohm.
6.11 Warranty and conformity 6.11.4 Quality Management Principles Metrohm Ltd., CH-9101 Herisau, Switzerland CH-9101 Herisau/Switzerland E-Mail info@metrohm.com Internet www.metrohm.com Metrohm Ltd. holds the ISO 9001 Certificate, registration number 10872-02, issued by SQS (Swiss Association for Quality and Management Systems). Internal and external audits are carried out periodically to assure that the standards defined by Metrohm’s QM Manual are maintained.
7 Index 7 Index A Accessories ..........................327 Acoustic signal........................37 Parameters ..................286 Action ......................................42 Result limits .................241 Add fixed volume ..................181 ADD parameters ...................270 Additional evaluation ............231 Adjustment data Swing Head ...................63 USB Sample Processor.60 Administrator rights.................27 Air bubble..............................317 Ambient temperature .
7 Index CTRL parameters ................. 278 Curve ............................ 139, 154 Curve Simulator 822 ............. 301 Cylinder Serial number ................ 44 Volume........................... 44 D Data card .......................... 78, 83 Date ........................................ 23 Decimal places Measured value display 36 Delete Command.................... 113 Common variable .......... 92 Device............................ 55 File ................................. 80 Method ...........
7 Index Export List of measuring points .....................................142 Results .........................142 Sample data ................142 Extension cable.....................328 External position .......61, 62, 189 Rinse position ................62 Shift position ..................62 Swing angle ...................61 Work position.................61 F FDA Guideline 21 CFR Part 11 ..........................................31, 34 File Copy ..............................81 Delete..................
7 Index Insert command .......... 115 Load ...................... 22, 107 Note ............................. 122 Options ........................ 116 Parameters .................. 193 Properties .................... 123 Sample data ................ 119 Save............................. 125 Sign ............................. 116 Signature ....................... 27 Start options ................ 121 Statistics ...................... 118 Stop options ................ 121 Template......................
7 Index Remote box...............56, 57, 186 Pin occupancy .............307 Remote lines .........................278 Remove PCMCIA card..........302 Rename...................................82 Report ...................................254 Audit trail................36, 173 Calculations .........170, 256 Common variables ......173 Curve ...................170, 255 Custom calibration buffers .....................................173 Delete...........................254 Devices ................
7 Index SET ....................................... 194 Parameters .................. 206 Troubleshooting .......... 289 Setting lines Parameters .................. 278 Settings Control ........................... 22 System-specific ............. 23 Sign Determination ........ 28, 135 Method .................. 27, 116 Signature Command.................... 286 Delete .................. 117, 135 Reasons ........................ 31 Signature line ................ 169, 255 Size ...............................
7 Index Sample.........................126 USB Lab Link ..........................72 USB Sample Processor .58, 187, 280 Adjustment data ............60 Calibration ...........258, 266 Tower 1 ..........................60 Tower 2 ..........................60 Troubleshooting...........293 User ........................................22 Administrator rights .......27 Deactivate......................27 Delete.............................26 Dialog ............................27 Edit...............................
