CH-9101 Herisau/Switzerland Tel. +41 71 353 85 85 Fax +41 71 353 89 01 E-Mail sales@metrohm.ch Internet http://www.metrohm.ch 774 Oven Sample Processor Instructions for use Program version 5.774.0010 8.774.1043 2005.
Table of contents Page 1 Overview 1.1 1.2 1.3 2 2.5 3 3.2 3.3 23 Configuration _____________________________________________ 23 3.1.1 Basic settings ............................................................................. 23 3.1.2 Oven settings .............................................................................. 24 3.1.3 Rack definitions .......................................................................... 25 3.1.4 Dosing units ....................................................
Table of contents Page 5 Detailed description 5.1 5.2 43 The display ________________________________________________43 The keyboard ______________________________________________44 5.2.1 Individual key functions .............................................................. 45 5.2.2 Data entry ................................................................................... 59 5.2.3 Text Entry .................................................................................... 60 5.
Table of contents Page 6 Appendix 6.1 6.2 6.3 6.4 6.5 6.6 6.7 6.8 7 137 Error messages __________________________________________ 137 Technical data____________________________________________ 140 Maintenance and servicing ________________________________ 142 6.3.1 Maintenance / service............................................................... 142 6.3.2 Servicing / care .........................................................................
1.1 Application range 1 Overview 1.1 Application range The Metrohm 774 Oven Sample Processor is a very versatile instrument. It has been specially designed for laboratory use and can be used for a wide range of applications. It provides an essential service when large numbers of samples have to be processed in which the samples require to be heated and/or whenever it is necessary to remove moisture or organic solvents from solids or liquids by the application of heat.
1 Overview also be used for demanding special applications as well as for routine tasks. The operating sequences for processing individual samples can be freely defined within wide limits. The same applies to the start and final sequences, which always need to be carried out once before the start and once at the end of a sample series. A learning mode is provided for the creation of operating sequences; with its help command parameters can be set manually.
1.3 Instrument description 1.3 Instrument description 1.3.
1 Overview 1.3.2 Oblique view from left-hand side with protective cover in position Gas supply Flow regulator Protective cover Inert gas inlet Sample rack with grip Drying flask connections Holder for drying flask Oven with protective jacket Drying flask with molecular sieve Safety information: The protective cover and the plug cover have to be in position for safety reasons. The plug cover prevent spilt solvents or chemicals from adversely affecting the connections and interfaces.
1.3 Instrument description 1.3.3 Rear view Gas supply Air inlet filter Flow regulator Outlet heater / transfer tube Inert gas inlet Sample rack Plug cover Drying flask Rear socket strip Type 1.774._ 0000/ 00 00 External Bus Address RS 232 Keyboard Made by Metrohm Herisau Switzerland 1.3.4 The socket strip (rear panel): Serial number Type 1.774.
1 Overview 1.3.5 Guide head Gas supply (gas inlet) Heated transfer hose (outlet heating) Needle adapter made of PEEK Hollow needle with Luer connection (exhaust) Guide rod (adjustable) Hollow needle (injection needle) Infrared sensors 1.3.6 Sample rack The tower of the 774 Oven Sample Processor is equipped with infrared beaker sensors which detect the presence of a vial in front of the tower. This "beaker test" is carried out after every MOVE command. Special position 1 (for conditioning vial) d.
1.3 Instrument description When the sample rack is positioned the rod magnets on the base of the rack are read in automatically. The arrangement of the magnets defines the rack code, which is allocated to an internal position table with whose help the 774 Oven Sample Processor recognizes the arrangement of the vial positions on the rack. The above arrangement corresponds to the magnet code 000001. 1.3.7 Sample vials The sample rack (order no. 6.2041.700) is intended for use with sample vials (order. no.
2 Installation 2 Installation 2.1 Setting up the instrument Packaging The 774 Oven Sample Processor is supplied with the accessories in separate special packages designed to ensure maximum protection. These contain shock-absorbing foam linings. As only these special packages guarantee damage-free transport of the instrument, it is essential you store them in a safe place.
2.2 Power supply • Checking and replacing fuse Carefully remove the built-in fuse and check its specifications. (The position of the fuse in the fuse holder is marked by the white arrow printed next to the supply voltage): 2.0 A (slow) ord. no. U.600.0019 • Replace fuse Replace fuse if necessary and reinsert it in the fuse holder. • Insert the fuse holder Insert the fuse holder according to the appropriate supply voltage.
2 Installation 2.3 Safety considerations • Do not operate the 774 Oven Sample Processor without protective covers. The plug cover protects the connectors from spillage. Organic solvents are always a potential serious fire hazard. The protective cover of the guide head prevents the access to the stroke path of the injection needle. Never get your hand beneath the protective cover while operating the instrument.
2.4 Arranging the accessories If opening the instrument is unavoidable, the following safety precautions are to be strictly adhered to: Before opening the instrument disconnect it from all electrical sources. Make sure that the power plug has been pulled out. Only in exceptional cases should the instrument be opened while it is switched on. Because parts that conduct current are exposed in this case, this should only be undertaken by an expert who is acquainted with the associated dangers.
2 Installation 2.4.2 Equipping the guide head • Screw the needle adapter (6.1808.150) onto the bottom of the guide head. • Attach the outlet hollow needle (6.2816.060) to the Luer connection of the needle adapter. Guide head Needle adapter Hollow outlet needle Hollow injection needle • Carefully introduce the hollow injection needle (6.2816.050) into the guide head from above (see arrow). Pull the needle downwards to the full extent. • Now lead the gas inlet (6.1805.
2.4 Arranging the accessories 2.4.4 Adjusting the needle position Allen screws In addition to the adjustment of the sample rack, the position of the needle (radial positioning) may be adjusted. After the adjustment of the sample rack proceed as follows: 1. Place a sealed beaker under the needle. 2. Lower the needle on to the seal. 3. Loosen the Allen screws of the sliding devices. 4. Position the needle in the centre of the seal. 5. Fasten the sliding devices. 6. Press .
2 Installation 2.4.5 Installation of the tubing system and the drying flask A stream of gas with a constant flow rate is required to transfer the moisture which is released when the sample is heated to a measuring vessel. You can either use the built-in pump to supply air or use an inert gas such as nitrogen for this purpose. Inert gas connection Connect the inert gas to the 'Air/N2 in' connection on the left-hand side of the instrument. Make sure that the pressure in the supply line is less than 1 bar.
2.5 Integration 2.4.6 Installation of the measuring cell Example: 6.1464.320 Coulometer titration vessel Transfer hose with outlet heating Connection for outlet heating Outlet heater Generator electrode with drying tube Indicator electrode Install the necessary accessories as shown in the diagram alongside. The fastening screws can be used to permanently fix the whole assembly in position.
2 Installation The 774 Automation System 700 Dosino 685 Dosimat 756 Coulometer 684 737 729 PC software Coulometer 729 Dosimat Interface 701 ... External Bus 784 Titrino family Metrohminstruments other instruments Remote RS 232 726 Titroprocessor printers Seiko Citizen Epson HP IBM … other instruments 774 774 Oven Sample Processor 2.5.1 Remote connections 774 Oven Sample Processor — 756 Coulometer for coulometric determinations 6.2125.110 cable (RS232) 756 774 6.2141.
2.5 Integration Control commands of the 774: CTL:Rm : START Gerät1 CTL:Rm : *************1 CTL:RS &U.R.N CTL:RS "774BLANK"..$G starts Coulometer " loads a method in the Coulometer here e.g. "774BLANK" Scanning the remote lines of the 774: SCN:Rm SCN:Rm : : **0**010 *****000 waits for 'cond. ready' waits for end of determination 774 Oven Sample Processor — 737 Coulometer for coulometric determinations 737 774 6.2141.
2 Installation Control commands: CTL:Rm : START Gerät1 CTL:Rm : ***********1** starts Titrino advance impulse / ENTER Scanning via remote lines: SCN:Rm : SCN:Rm : ****1000 *****010 waits for end of titration (EOD-impulse) waits for 'cond. ok' In principle it is possible to use an additional RS232 connection to automatically load a particular method in the Titrino while a sequence is being processed. Please refer to the example of the remote connection given for the 756 Coulometer on the previous page.
2.5 Integration 2.5.2 External bus connections If a KF Titrino or a Coulometer which does not support automatic solvent changing is connected to the 774 Oven Sample Processor then this can be carried out with the help of a 700 Dosino. 685 Dosimats can also be used for the addition of solvents. 700 Dosinos or 685 Dosimats are connected to the 774 Oven Sample Processor via the so-called 'External Bus'. A 729 Dosimat interface can be used to connect up to 4 dosing devices to the 'External Bus' interface.
2 Installation 2.5.3 Serial connection (RS232) Many different instruments may be connected via the serial RS232 interface. In addition to all Metrohm instruments that support the Metrohm remote control language (see page 101ff) any printer with serial interface (or parallel interface and parallel/serial converter) or a personal computer (PC) may be connected. Any other measuring instrument may be controlled via RS232 interface, as long as it supports serial data transmission. 6.2125.
2.5 Integration 2.5.4 Connecting a printer Printers with the following printer emulations may be connected: IBM Epson Seiko Citizen HP IBM Proprinter and printers with IBM emulation Epson printers and printers with Epson emulation Seiko printer DPU-411/414 Citizen printer IDP560 RS HP printers and compatibles with HP PCL3 emulation If you connect a printer not listed in the following table, be sure that it is able to emulate Epson or IBM Proprinter mode. Use the 6.2125.
2 Installation Printer type Cable RS232 Settings Settings on Printer Citizen IDP560-RS 6.2125.050 baud rate: 9600 data bit: 8 stop bit: 1 parity: none handshake: HWs character set:Citizen DIP switch settings: on off 1 2 3 4 5 6 7 8 The 7-bit ASCII character is altered to the specific national character set by setting the jumpers J1 and J2 as follows: J1 open closed closed.
3.1 Configuration 3 Introduction 3.1 Configuration The 774 Oven Sample Processor must be configured correctly before it is used for the first time. This includes both the basic settings with the oven settings and the configuration of the sample rack and the peripheral devices which are connected. All these settings are accessible via the configuration menu which can be opened with the key. It is arranged in various submenus according to subject.
3 Introduction device label In order to be able to identify each particular laboratory instrument unambiguously (required by GLP) the sample changer can be given an 8-character identifier made up of letters and/or numbers. Text input is described on page 59. program version The program version (instrument software) cannot be altered. It is shown in the configuration menu for information. max. lift way The maximum lift way is an important safety entry.
3.1 Configuration 3.1.3 Rack definitions The 774 Oven Sample Processor is supplied with the standard rack for 35 samples. The rack positions for this rack (Rack 1) are already preconfigured. Sample position 36 is reserved for a conditioning beaker. If different configurations are to be defined for the same type of rack then the individual racks must be allocated different codes and the stud magnets on the base of each sample rack arranged accordingly.
3 Introduction shift position The sample rack can only be rotated when the lift is at or above the shift position height. The shift position should therefore be selected so that safe rotation of the sample rack is always possible, i.e. it must be impossible to damage either the needle or the rack when the rack is rotated. Please note that the conditioning vessel is slightly higher than the other sample vessels.
3.1 Configuration tubing lengths and diameters These values are only relevant for the 700 Dosino. As this has the ability to prepare the complete tubing system automatically for dosing, i.e. to rinse the tubings and fill them with dosing solution, the particular tubing lengths and (inner) diameters must be entered. The necessary rinsing volumes are then calculated automatically. The settings for dosing units mentioned above must be carried out for all 4 ports of the 700 Dosino (inlets and outlets 1–4). 3.
3 Introduction 3.1.6 Lock keyboard functions Particular areas of the operator dialog can be made inaccessible to untrained operators by locking individual dialog areas or keys. In this way the accidental overwriting of a method or even the alteration of parameters can be prevented. The menu '>keyboard options' for the corresponding functions is opened by holding down the key when the Oven Sample Processor is switched on.
3.1 Configuration lock display If the Oven Sample Processor is to be operated solely by external control software (see above) then the display for manual operation can be switched off. 'lock display: on' locks the display.
3 Introduction 3.2 Manual operation As an introduction only those basic manual control functions which are necessary for preparing the sample changer for processing a series of samples are described here. Only a few keys are required. For further commands and details please refer to page 61ff and page 74ff. Shift sample rack / position samples The <Í> and <Î> keys can be used to rotate the sample rack one position to the left (counterclockwise) or right (clockwise).
3.2 Manual operation Set sample position SAMPLE 7 The SAMPLE function is used to set the current sample position. It defines the first sample beaker for the following series of samples. Pump / Valve FLOW 4 The FLOW function is used for switching the pump or inert gas solenoid valve on and off.
3 Introduction The first parameter of the DOS command represents the number of the dosing instrument (1–12), the second parameter the function or volume to be dosed. Example: DOS: 2 DOS: 2 4.51 ml
3.3 Methods and Sequences 3.3 Methods and Sequences 3.3.1 Designing a method A method is made up of the following components: • number of samples to be processed • run sequences (start, sample and final sequences) • Definition of the various instrument settings (report definitions, sample changer settings, time-out settings, gas flow settings, dosing unit definitions, manual stop options) For details about instrument settings please refer to page 67ff.
3 Introduction Sequences are created in the submenus '>start sequence', '>sample sequence' and '>final sequence'; these can be accessed via the parameter menu (press ). A sequence is arranged in lines. If a command is entered a new line containing this command will be appended to the line which is currently shown. The line number can be seen in the display. 99 lines are possible per sequence. A line is deleted by pressing . The following lines move up one position.
3.3 Methods and Sequences The LEARN function is available for the following commands: Command Adaptive parameter Type of function LIFT WAIT DOS SCN Rm SCN RS absolute additive additive "live" value "live" value Lift position in mm pause time in seconds Dosing volume in mL Status of the 8 remote lines Received character string TRACE function The "TRACE" function is a valuable aid for processing a complete sequence or method, or excerpts, step-by-step for test purposes.
3 Introduction 3.3.4 POWER-UP methods When the 774 Oven Sample Processor is switched on the sample rack and the guide head move to their rest positions. In order to condition the complete carrier gas tubing system when the instrument is switched on a "POWER-UP" method can be used. This method is automatically started when the instrument is switched on.
4.1 Oven control 4 Oven control and gas flow In addition to the essential sample changer features, such as rotating the sample rack and raising and lowering the lift, the 774 Oven Sample Processor also has a controllable sample heating block and a gas supply device. This means that it is extremely suitable for applications in which moisture or solvent vapors are to be driven out of a sample at an increased temperature and transferred to a measuring cell in a stream of carrier gas.
4 Oven control and gas flow • Programmable HEATER command – the HEATER command can be used as a part step in the processing sequence of a method. This means that it is possible to alter the program-controlled oven temperature whenever this is necessary. If the HEATER command is used the heating-up period can be freely selected so that it is possible to carefully warm up a sensitive sample. Temperature profiles or ramps within a sequence can be followed by repeated use of the HEATER command.
4.2 Gas flow Gas flow diagram: air inlet pressure control valve inlet filter pump gas flow control knob conveying tubing inert gas inlet Air/N2 in outlet needle solenoid valve to Drying flask flow meter injection needle from Drying flask titration cell sample tower Gas flow left-hand instrument side Air/N 2 in The gas flow can be set manually with the help of the gas flow regulator and the flowmeter.
4 Oven control and gas flow 4.3 KF Moisture determination The 774 Oven Sample Processor is predestined for Karl Fischer moisture determinations. The oven method is used for those samples in which the direct determination of the water content is either impossible or very difficult. This applies for substances which either directly react with the Karl Fischer reagents or only release their moisture very slowly into the reaction solution because of their insolubility, e.g. plastic granulates or oils.
4.3 KF Moisture determination water [µg] The blank value is made up of the moisture which adheres to the sample vial * and a system drift which is latently present and whose cause can be found in a minimal residual moisture in the carrier gas and possibly leaks in the tubing system. total blank value system drift in µg/min vial humidity in µg min. extraction time t [min] determination interval drift [µg H2O/min] *The use of pre-dried sample vials has no significant advantages.
4 Oven control and gas flow Evaluation The water determination as such can be carried out with a Coulometer or Karl Fischer titrator. If a Coulometer is used care must be taken that gas flow and oven temperature are selected so that the sample moisture is not driven off too quickly. Otherwise a moisture excess may not be absorbed by the solvent in the Coulometer cell, but condense in the upper part of the cell or even be blown out of the cell.
5.1 The display 5 Detailed description 5.1 The display The display consists of two lines, each having 24 characters. The first line serves as a title line in which the current method and the sample counter reading are displayed. In edit mode the menu title is shown. The second line serves as a status line which displays specific activities depending on the operating state. In edit mode it serves as an entry line.
5 Detailed description 5.2 The keyboard Metrohm 774 SC Controller HEATER CONFIG FAN PARAM PUMP U SER METHOD SAMPLE HOME INSERT DELETE END DISPLAY RESET SELECT CLEAR QUIT VALVE ENTER MOVE LIFT 7 8 9 FLOW HEATER DOS 4 5 6 SCAN CTRL WAIT 1 2 3 DEF PRINT 0 . < RACK > * LEARN HOLD STOP START 6.2142.030 Most of the keys have two functions according to whether the sample changer is in the normal state or in edit mode.
5.2 The keyboard 5.2.1 Individual key functions Key CONFIG PARAM Normal state Editing Opens the configuration Menu Select configuration settings • The key opens the selection menu for the configuration of the sample changer. • The settings in the Configuration Menu remain constant until they are changed or the working memory (RAM) is reinitialized. • When the Configuration Menu is open, pressing the key displays the next menu line.
5 Detailed description Key END Normal state Editing Lift in work position Select the last line of a menu • The key runs the lift of the active tower into the work position. • With the key, the last line in a menu or a sequence can be accessed. The work position is defined separately for every sample rack in the Configuration Menu under “>rack definitions”. • Any data that has been altered in a menu or command line is not carried over. See key.
5.2 The keyboard Key Normal state Editing Turn rack right Move the cursor one column to the right • The <Î> key turns the sample rack one position to the right, i.e. in the clockwise direction. The next lowest beaker position is placed under the lift. • The turning speed of the rack can be defined in the Parameter Menu or with the key. • With the <Î> key the cursor is moved one column to the right in an editing line with two parameters.
5 Detailed description Key DISPLAY SELECT Normal state Editing Selection of the display mode Select parameter • The display can be switched over to display of the measured values (oven temperature and gas flow) with key . Pressing this key again switches back to the previous display mode. This can be done in the basic state and whilst the method is running. • With the
5.2 The keyboard Key QUIT Normal state Editing Abort current command Abort Entry • Whilst a method is running, you can abort a command currently running with the key and continue with the next command. This is practical if a programmed waiting time is to be shortened or, in the case of a SCAN command, the expected signal cannot be recorded. Quit error messages • acknowledges error messages. During method processing the sample changer goes into the 'HOLD' state after this.
5 Detailed description Key SAMPLE 7 Normal state Editing Set sample position Numerical entry ('7') • The key serves to set the current sample position. or • If the current sample position is not manually set before the start of a sample series, rack position 1 is always started first. • In a start sequence the SAMPLE command serves to define the first sample of a sample series.
5.2 The keyboard Key FLOW 4 HEATER 5 Normal state Editing Activating/deactivating gas flow Numeric entry ('4') • Key is used to activate resp. deactivate the air pump or the solenoid valve (Air/N2 in). activate/deactivate gas flow or • The FLOW command serves to activate resp. deactivate the air pump or the solenoid valve (Air/N2 in). • The first parameter serves to select pump or valve. The second parameter defines status 'On/Off'. The function must be confirmed with .
5 Detailed description Key SCAN 1 Normal state Editing Display input signals Numerical entry • Display of the incoming signal or data on the remote or RS interface. This function serves to control the data communication or states of connected instruments. or • The first parameter represents the interface selection. The signals for data being received at that moment are displayed as the second parameter.
5.2 The keyboard Key Normal state Editing Parameters for the RS 232 interface • Character string with up to 14 alphanumerical characters. Default value: “&M;$G”, may be set with . Most Metrohm instruments can be controlled with such remote control commands, see pages 101ff. Numerical entry ('3') WAIT 3 or Define waiting time • Waiting for a certain time interval to elapse. DEF 0 Redefine various instrument settings • This function serves to temporarily change various settings.
5 Detailed description Key Normal state and editing • DEF commands are valid for manual operation as well as for the programmed processing of a method. • The individual DEF commands are listed below. DEF 0 DOSRATE DEF 0 FILLRATE Change dosing rate • The dosing rate may be individually set for every dosing drive (Dosimat or Dosino). • Syntax: DOSRATE [Dosing unit] [Dosing rate] Change filling rate • The filling rate may be set individually for every dosing drive (Dosimat oder Dosino).
5.2 The keyboard Key DEF 0 SHIFTRATE Normal state and Editing Change turning speed and direction • In addition to giving the turning speed of the sample rack in angular degrees/sec., the turning direction can also be indicated with the first parameter. • Turning direction "+" causes the sample beakers to be processed in the counterclockwise direction, i.e. in ascending order. Turning direction "–" indicates in the clockwise direction, i.e. in descending order.
5 Detailed description Key PRINT . < Normal state Editing Print report Text entry • The key serves for the manual printout of reports. • In a menu or sequence line in which entry of text is required, (for ex. method name), text edit mode is activated with "<". • Existing text is deleted in this event and the text cursor is set on the left margin of the text field. • "<" serves also for shifting the chain of characters to chose from, i.e.
5.2 The keyboard Key START Normal state Editing Start a Method Trace function • The key starts a method. Starting is only possible when the 774 Oven Sample Processor is in the normal state, i.e. when ‘ready’ is shown in the display. • During editing of a sequence, the command defined in the command line can be directly executed with the key. • When starting a sample series, the sample counter is set to 0.
5 Detailed description Key Normal state Editing LEARN Interrupt Process Switch on LEARN mode HOLD • The key interrupts the processing of a method. However connected peripheral instruments (Titrinos, etc) are not halted. Only method processing is interrupted. • The key serves to start the Learn mode. This mode is provided for easier editing of process sequences. It allows direct acceptance of a parameter value that has been set by manual control.
5.2 The keyboard 5.2.2 Data entry Edit line In a menu line or a sequence one or two parameters respectively can be entered. A blinking block cursor indicates where a parameter can be entered. >changer settings shift rate ¦ 20 Ï Í title line Í edit line Ï Ï menu item cursor parameter >sample sequence 08 FLOW: ¦ pump Ï command : on Í title line Í edit line Ï Ï first parameter, second parameter The cursor keys, <Î> and <Í>, can be used to switch between the parameters.
5 Detailed description 5.2.3 Text Entry The text editor can be used when text entry is provided. Numbers can be entered directly via the keyboard. PRINT . < RACK *- The keys "<" or ">" open the text editor. With "<" an existing character > string is deleted and the text cursor is set to the left margin of the edit line. With ">" an existing character string remains and the text cursor is set on the last character of the existing text.
5.2 The keyboard Scheme: >store method method: ******** "<" or ">" blinking text cursor character chain >store method █ ABCDEFGHIJ...abcd...1234...*%&/()=... method: 2x ">" blinking text cursor >store method method: █ CC DEFGHIJ...abcd...1234...*%&/()=... "<" or ">" ...... >store method method: Chloride reject accept An entire text line can be entered in this way, for example, for the naming of a method. Text editing can be ended with .
5 Detailed description 5.
5.3 Menu organization CONFIG 5.3.
5 Detailed description >auxiliaries beaker sensor: ON ON,OFF configuration >oven settings Submenu of oven settings Open submenu with >oven settings initial temp.: Use to access next higher level Activate or deactivate beaker sensor OFF °C OFF, 50…250 °C >oven settings max.temperature 275 °C Setting the initial temperature of the oven after switching on OFF = Do not switch on oven heater Maximum possible temperature (overheating safeguard) 50…275 °C >oven settings temp.
5.3 Menu organization >rack definitions work position 1 0 mm 0…100 mm Working position of the lift (in mm from the upper stop) The working position is used for sample determinations Pressing directly accepts the current lift position. >rack definitions rinse position 1 0 mm 0…100 mm Rinsing position of the lift (in mm from the upper stop) The rinsing position is used for the conditioning vessel Pressing directly accepts the current lift position.
5 Detailed description >dosing units max. rate 1 use to access the next highest level 1 160 ml/min Max. dosing speed (depends on burette size) 0.01…160 ml/min >dosing units 1 tube length 1 1000 mm 0, 1000, 30000 mm Length of the tubing on Dosino port 1 >dosing units tube diameter 1 Diameter of the tubing on Dosino port 1 1 2 mm 0.1…2.0…20 mm >dosing units max. rate 2 1 160 ml/min Max. dosing speed (dependends on burette size) 0.01…160 ml/min >dosing units ...........................
5.3 Menu organization The settings for the printers recommended by Metrohm are listed on page 20f. For printers not listed, the setting “Epson” is recommended. In any case the printer handbook should be consulted. For data transfer with personal computers, “IBM” must be chosen. >RS232 settings RS control: ON Switch remote control on and off ON, OFF If the remote control is switched off, no data can be received, however reports can still be printed.
5 Detailed description PARAM 5.3.2 Parameters All settings of the Parameter Menu constitute a method and may be saved as such. Main Menu: parameters number of samples rack 1…999, rack,* Number of samples to be processed rack * = one entire rotation of the rack = infinite number of samples All sample positions of an engaged rack will be processed when the instrument is on the ‘rack’ setting. (max. number of rack positions – number of special beakers defined).
5.3 Menu organization parameters >start sequence Editor for the start sequence of a sample series Open the submenu with The sequence entered here is run once when a sample series is started. This may be used to process blind samples for instance. parameters >sample sequence Editor for processing sequence for each sample Open the submenu with This sequence is run when processing each individual sample of a series.
5 Detailed description parameters >report Submenu for report type definition Open the submenu with >report report: none none fulll short config param usermeth all Setting of the report type = No report output = Output of the oven temperatures = Short result report = Listing of the device configuration = Method listing = List of all stored methods = Printout of all above reports When selecting a result report (full or short), a separate report is printed out for each sequence (start, sample and
5.3 Menu organization >changer settings on beaker error: MOVE MOVE, display Defining the reaction to a missing beaker MOVE = display = The last action will be executed once more. The next position according to the currrent SAMPLE command will be chosen. Processing will be interrupted and a warning displayed. If processing should not be halted when a sample beaker is missing, 'MOVE' can be chosen. In case of a missing beaker another MOVE command is executed with the next sample.
5 Detailed description 'EoD' (End of Determination) pulse at the remote link. The SCAN timeout defines the maximum permitted duration of a determination in this case. The timeout time starts directly on activation of the SCAN command. After the timeout time has expired, an error message is displayed and the sequence of the method is aborted (HOLD status) or the system continues with the next command of the sequence, depending on the setting above.
5.3 Menu organization Parameter >dosing unit def. Submenu for dosing unit settings Open the submenu with >dosing unit def. dosing unit 1 Select dosing unit 1…12 After entering the address of the dosing unit and confirming with it will be displayed in the first menu line. >dosing unit dos.rate: 1 160 ml/min 0.01…160 ml/min, max. >dosing unit 1 fill.rate: 160 ml/min Set the dosing speed Set the filling speed 0.01…160 ml/min, max.
5 Detailed description parameters >manual stop Submenu for defining reaction to manual stop Open the submenu with The following entries define the commands to be executed when the key is pressed. This allows connected peripherals to be stopped automatically or the functions of the 774 Oven Sample Processor to be reset.
5.3 Menu organization USER METHOD 5.3.
5 Detailed description 5.4 Command reference The following commands are programmable within a sequence. Most of them are also available in manual operation but may vary partially in their operation or exhibit a limited parameter selection; see page 31ff. The following listing is valid for the programming of process sequences.
5.4 Command reference settings” the turning direction and speed can be defined specifically for each method. These can also be modified in a sequence with the corresponding ‘DEF’ command. If there is no vial in the rack position chosen, this is recognized by the beaker sensor. The changer reaction to a missing vial can be predefined in the Parameter Menu under ">changer settings". The alternatives available are halting the processing and issuing an error message or selecting the next rack position.
5 Detailed description FLOW FLOW 4 >sample sequence 4 FLOW: pump pump, valve Gas flow control : ON ON, OFF The FLOW command can be used to activate resp. deactivate the pump (air) or the solenoid valve (inert gas input). The first parameter is used to select pump or valve. The flow rate of the carrier gas stream can be controlled in both cases with the flow controller on the left-hand side of the tower of the 774 Oven Sample Processor. The flow rate is measured and monitored electronically.
5.4 Command reference DOS DOS 6 Dosing Control >sample sequence 06 DOS 1 : 1 ml 1…12,* fill, release, prepar., empty, 0.001…1…999.999 ml The DOS command is used to control Dosimats and Dosinos. Up to 12 Dosinos or Dosimats can be addressed via the External Bus control. In addition to adding a certain volume, specific actions can be initiated. fill release prep empty Filling the Dosimat or Dosino burette Prepare Dosimat or Dosino for changing the exchange unit. Burette is filled via the rinsing port.
5 Detailed description Setting special bit patterns allows flexible control of connected instruments. Here the following is valid: Example: 0 = line inactive 1 = line active * = arbitrary line state 00000001 = input 0 is active = instrument 1 "Ready" The bit pattern (= line state ) can be taken over interactively with the LEARN function. See page 34. Details about the remote interface are found on page 97.
5.4 Command reference CTL CTRL 2 Setting the remote lines >sample sequence 9 CTL:Rm START device1 Rm START device1 START Dos1 STOP device1 START 737 ENTER INIT = start instrument 1 = start Dosimat on instrument 1 = stop instrument 1 = start Coulometer 737 = simulate key = initialize remote interface 14 Bit (1,0 oder ∗) arbitrary 14 bit pattern The CTL:Rm command controls external instruments via the remote interface.
5 Detailed description This function is suitable for instruments with Metrohm remote control language. These can be controlled with so-called triggers. The most important of these are: &M;$G &M;$S &M;$H &M;$C Go, start instrument in current mode Stop, stop instrument Hold, interrupt method Continue, resume method The following remote control commands can switch on the AutoInfo status messages of a Metrohm instrument (for example, in a start sequence): &Se.A.T.R"ON" &Se.A.T.F"ON" &Se.A.T.S"ON" &Se.A.T.
5.4 Command reference DEF DEF 0 Redefining specific instrument settings During method processing the most diverse settings can be made using the following DEF commands. The individual entries are accessed by repeatedly pressing the DEF key (roll-up selection). >sample sequence 14 DOSRATE 1 Dosing speed 160 1…12 0.01…160 ml/min The dosing speed for all 12 dosing units can be individually set.
5 Detailed description >sample sequence 18 DRIVE.PORT 1.1: dos. 1.1…12.4 Dos. fill, rinse, prep., drain Port assignment for the 700 Dosino = Dosing = Filling = Rinsing = Preparation = Emptying The port assignments of a 700 Dosino can be changed as needed. The first parameter stands for the dosing unit and inlet or outlet port of the Dosino. The dosing unit and the port must be separated by a period. The four ports (1-4) of every 700 Dosino can therefore each be designated a function.
5.5 Printing reports 5.5 Printing reports You can have reports printed out directly by the 774 Oven Sample Processor for documentation purposes. However, this does necessitate connecting a printer with serial port to the RS232 socket. This means that no direct RS232 connection to a Metrohm Coulometer 756 is possible. Please refer to Page 20f for details of how to connect and configure a printer.
5 Detailed description 0 s 120.9 10 s 121.9 20 s 122.7 30 s 121.9 40 s 120.7 50 s 120.5 ... ... 350 s 121.1 360 s 121.1 370 s 120.7 ============ °C °C °C °C °C °C Å Oven temperatures, intervals in accordance with 'recording interval' °C °C °C The values listed each refer to the part-sequence currently being processed or processed last (start sequence, sample sequence or final sequence) of the method Configuration report 'co 774 Oven Sample Proc. 0130/03 5.774.
5.5 Printing reports Parameter report / method 'pa 774 Oven Sample Proc. 0130/03 parameters method 756Pump number of samples: rack >start sequence 1 CTL:Rm: INIT 2 MOVE 1 : spec.1 3 CTL:Rm: START device1 4 HEATER:INIT°C 5 LIFT: 1 : rinse 6 FLOW: pump : ON 7 WAIT 300 8 SCN:Rm : Cond ok >sample sequence 1 MOVE 1 : spec.
5 Detailed description Method memory report 'um 774 Oven Sample Proc. 0130/03 5.774.0010 user memory >methods Titrino 1304 756Pump 1216 756Valve 1216 756Coulo 2680 737Coulo 1144 KF+Exch 1696 remaining bytes 17720 ------------ Å Report identification ('um = user methods) Å Report title with device number and program version Å List of stored methods Å Memory space still available 5.5.1 Automatic reports You can choose the type of report in the Parameter menu. Only one report can be defined at any one time.
5.6 Sample racks 5.6 Sample racks A sample rack is a turntable for accommodating sample vials. The standard sample rack supplied with the 774 Oven Sample Processor can be detached to insert samples and can then be fitted back on again. It is designed for 35 sample vials whose dimensions must correspond to the specifications so that these vials (22 mm Head Space Vials, order No. 6.2419.000) fit precisely in the oven's opening. The arrangement of the sample positions on the rack is defined in a rack table.
5 Detailed description The following recognition data can be defined for each rack: Rack number Code Type Work position Rinse position Shift position Special position Special beaker position unique identification automatic rack recognition racktype / position table working height of the lift head rinsing height of the lift head turning height of the lift head freely available lift position reserved beaker positions (spec.1 to 8) The Rack number serves to identify a rack. It can be chosen from 1 to 16.
5.6 Sample racks Special beakers Special beakers are reserved positions of a sample rack. 0 to 8 special beakers (1 special beaker as conditioning vial as the default setting) per rack can be defined. They can be positioned in front of the tower in a method sequence for specific operations without interrupting or obstructing the sequence of the sample series. Special beakers may be used to schedule special functions for a conditioning vessel. Special beakers are placed under the lift with "MOVE 1 : spec.
5 Detailed Description 5.7 Dosimats and Dosinos 685 Dosimats and 700 Dosinos can be connected as dosing units to the "external bus" socket. An E-bus cable and a 729 Dosimat Interface are required for this. Four dosing units can be operated on one interface. Three Dosimat Interfaces can be linked serially (cascaded, observe address, see page 19). This makes it possible to connect 12 dosing units simultaneously to a 730 Sample Changer and specifically address each of them with the 'DOS' command.
5.6 Dosimats and Dosinos The Dosino has five ports (inlets and outlets) which can be assigned various functions. Port 1 Port 4 Port 2 Port 0 Port 3 View of a Dosino from underneath Port 0 – serves as ventilation for the reserve bottle and is usually fitted with an absorber tube (filled with desiccant). Port 1 – is situated on the side and under standard operating conditions is defined as the dosing outlet.
5 Detailed Description The maximum dosing and filling rates that can be entered in the configuration menu under '>dosing units' for every port of a dosing unit depend on the burette size: Volume of the dosing unit 2 mL 5 mL 10 mL 20 mL 50 mL Max. dosing rate 7 mL/min 17 mL/min 33 mL/min 67 mL/min 160 mL/min Resolution 0.2 µL 0.5 µL 1.0 µL 2.0 µL 5.0 µL The following commands can be executed with Dosinos.
5.6 Dosimats and Dosinos calculated from the configuration settings for tubing length and diameter (see page 66f). Under standard conditions the tubings are emptied via the dosing port. However this can be changed by the following commands. >dosing unit def. preparation XX port Y or DRIVE.PORT XX.Y : prep. Emptying DOS: XX : empty mL Empty the dosing and filling tubes. The tubing system and the burette of the Dosino can be completely emptied.
5 Detailed Description Ejecting DOS: XX : eject mL Empty the Dosino burette. The contents of the burette is ejected completely via the dosing port. This can be redefined as desired (see Dosing). Adjust DOS: XX : adjust mL Compensate the play The mechanical play between the dosing piston and the spindle is compensated. This command is important for exact pipetting when small volumes are aspired into the pipetting tube and ejected again.
5.8 Remote Interface 5.8 Remote Interface Peripheral instruments connected such as Titrinos, Titroprocessors, Coulometers etc. can be controlled via the remote interface (25-pin socket). 14 lines (Output 0–13) are available for the emission of signals. For receiving signals (e.g. the "ready" signal of a Titrino at the end of a titration) 8 lines are provided (Input 0–7).
5 Detailed description The 14 output lines of the remote socket can be separately set (statically) in manual operation as well as during method processing with the "Control" command (CTL). A 14-place bit pattern must be defined for this. Every bit is assigned to an output line.
5.8 Remote Interface CTL-command Parameter Bit Pattern INIT START device1 START dos1 00000000000000 *************1 *******1****** STOP device1 START 737 ENTER Function initializes the remote interface starts device1 (for ex., Titrino, Coulometer...) starts Dosimat on device1 (Titrino via "activate", 6.2141.040 cable required) ************1* stops device1 (for ex., Titrino, Coulometer...) *********1**** starts Coulometer 737 (6.2141.
5 Detailed description 100 774 Oven Sample Processor, Instructions for use
5.9 Operation via RS232 Interface 5.9 Operation via RS232 Interface 5.9.1 General rules The 774 Oven Sample Processor has an extensive remote control facility that allows full control of the Sample Changer via the RS232 interface, i.e. the Sample Changer can receive data from an external controller or send data to an external controller. CR and LF are used as terminators for the data transfer.
5 Detailed description 5.9.2 Calling up Objects An excerpt from the object tree is represented below: 3rd node Language 2nd node Prog RSSet Aux 1st node Config Mode 0st node & Root Rules Example The root of the tree is designated by &. The branches (levels) of a tree are marked with a dot (.) when calling up an object. When calling up an object, it is sufficient to give only as many letters as necessary to uniquely assign the object.
5.9 Operation via RS232 Interface 5.9.3 Triggers Triggers initiate an action on the 730 Sample Changer, for example, starting a process or sending data. Triggers are marked by the introductory symbol $. The following triggers are possible: $G Go $S $Q Stop Query $Q.P $Q.H Path Highest Index $Q.N"i" Name $D Detail-Info $U qUit Starts processes, e.g.
5 Detailed description Detailed Status Conditions Status conditions of the global $R: $R.Mode $R.Assembly Basic state: ready to start automatic processing An assembly step has been executed. Status conditions of the global $G: $G.Mode.Start. $G.Mode.Start.01.WAIT $G.Mode.Sample.01.WAIT $G.Mode.Final.01.WAIT $G.Mode. $G.Assembly.
5.9 Operation via RS232 Interface E40 E41 E42 E43 E44 E45 RS Send Errors: DSR=OFF. No proper handshake for more than 1s. Exit: . Is the receiver switched on and ready to receive? DCD=ON. No proper handshake for more than 1s. Exit: . Is the receiver switched on and ready to receive? CTS=OFF. No proper handshake for more than 1s. Exit: . Is the receiver switched on and ready to receive? Transmission has been interrupted for at least 3 s with XOFF. Exit: send XON or .
5 Detailed description 5.10 The remote control tree 5.10.1 Overview The internal object tree can be divided into the following branches: & ├ Mode ├ Config ├ Info ├ Setup ├ UserMeth ├ Assembly └ Diagnose Root Method parameters Instrument configuration Current Data Setting the operating mode User-defined methods Component data Diagnostics program Detailed Description of the Main Branches: 5.10.2 &Mode Object Description Input range & Root ├ Mode : ├ .Method ├ .
5.10 The remote control tree : ├ .Finalseq │ ├ .1 │ │ ├ .Cmd │ │ └.∗ │ │ │ ∗ │ : │ └ .100 │ ├ .Report │ ├ .Assign │ │ │ └ .TDelta │ ├ .Changer │ ├ .RackNo │ ├ .L1Rate │ ├ .L2Rate │ ├ .ShRate │ ├ .ShDir │ └ .ModeSample │ ├ .TimeoutSet │ ├ .HTime │ ├ .HAction │ ├ .STime │ └ .SAction │ ├ .Gas │ ├ .UnitFlow │ ├ .MinFlow │ ├ .MaxFlow │ ├ .Select │ └ .Otherfac │ ├ .DosimatSet │ ├ .DosUnitNo │ ├ .1 │ │ ├ .DosRate │ │ ├ .FillRate │ │ ├ .DosTube │ │ ├ .FillTube │ │ ├ .ExchTube │ │ ├ .PrepTube │ │ └ .
5 Detailed description 5.10.3 &Config Object & Root Description : ├ Config Instrument configuration : ├ .Aux Miscellaneous │ ├ .Language Dialog language │ │ │ ├ .Contrast Display contrast │ ├ .Beeper Beeper on/off │ ├ .DevName Instrument identification │ ├ .Prog Program version │ ├ .MaxLift Max. Lift height │ └ .MonBeak Beaker sensor on/off │ ├ .OvenSet Ofen settings │ ├ .InitTemp Initial temperature │ ├ .MaxTemp max. temperature │ └ .TempCorr Temperature correction │ ├ .RackDef Rack definitions │ ├ .
5.10 The remote control tree : ├ .WetPart │ ├ .WetPartNo │ ∗ │ ├ .1 │ │ ├ .MaxRate │ │ ├ .Length │ │ └ .Diameter │ │ │ ├ .2 │ │ ├ .MaxRate │ │ ├ .Length │ │ └ .Diameter │ │ │ ├ .3 │ │ ├ .MaxRate │ │ ├ .Length │ │ └ .Diameter │ │ │ └ .4 │ ├ .MaxRate │ ├ .Length │ └ .Diameter │ └ .Rsset ├ .Baud │ ├ .DataBit ├ .StopBit ├ .Parity ├ .Handsh │ │ └ .CharSet Dosing unit definitions Dosing unit no. 1...12 Port number 1 Max. dosing rate Tubing length Tubing diameter 0.01...160 ml/min 0...1000...30000 mm 0...2...
5 Detailed description : └ .Errorlist ├ .1 : ├ .Time └ .ErrNo : └.10 : ├ .Results : ├ .TempSet ├ .LowTemp ├ .HighTemp ├ .Gasflow ├ .Lowflow ├ .Highflow └ .SmplHeatTime : └ .ActualInfo ├ .Meas │ ├ .CyclNo │ ├ .OvenTemp │ └ .Gasflow │ ├ .Lift │ ├ .1 │ │ ├ .Exist │ │ ├ .MaxHeight │ │ ├ .ActHeight │ │ └ .Beaker │ │ │ └ .2 │ ├ .Exist │ ├ .MaxHeight │ ├ .ActHeight │ └ .Beaker │ ├ .Rack │ ├ .Code │ ├ .Type │ ├ .WorkHeight │ ├ .RinseHeight │ ├ .ShiftHeight │ ├ .SpecialHeight │ ├ .ActPos │ └ .Act2Pos │ ├ .
5.10 The remote control tree : ├ .Heating │ └ .State │ ├ .Buret │ ├ .1 │ │ ├ .State │ │ ├ .Position │ │ ├ .Cock │ │ ├ .Type │ │ └ .Volume │ : │ └ .12 │ ├ .State │ ├ .Position │ ├ .Cock │ ├ .Type │ └ .Volume │ ├ .Inputs │ └ .Status │ ├ .Outputs │ └ .Status │ ├ .Display │ ├ .L1 │ └ .L2 │ └ .Counter ├ .Sample └ .Maximum Heater State read only 5.11.3.12 Dosing units Dosing unit 1 State Piston position Cock position Type of dosing drive Burette volume read only read only read only read only read only 5.
5 Detailed description 5.10.5 &Setup Object Description Input range Reference Settings for the operating mode Report identification Send key code Sending format of path info Short format of path Paths of modified nodes only on, off on, off on, off on, off Message on changed values on, off 5.11.4.
5.10 The remote control tree : : │ ├ .Heater │ │ ├ .T │ │ └ .S │ │ │ └ .E │ ├ .PowerOn ├ .Initialize │ └ .Select │ ├ .RamInit └ .InstrNo └ .Value Heater messages Changes of target temperature When heater is switched off on, off on, off When an error occurs on, off RESET (power on) Set default values Selection of branch $G $G param, config, assembly, setup, all $G 8 ASCII characters Initialization of working mem. Instrument number Description (not available in manual operation) 5.11.4.10 5.11.4.
5 Detailed description : ├ .Lift │ ├ .Station │ └ .Way │ │ ├ .Heater │ ├ .Temp │ └ .Time │ ├ .Flow │ ├ .Address │ └ .State │ ├ .Dos │ ├ .Address │ └ .Value │ │ │ ├ .Scan │ ├ .Address │ └ .Pattern │ │ │ │ │ ├ .Ctrl │ ├ .Address │ └ .Pattern │ │ │ │ │ │ ├ .Def │ ├ .Object │ │ │ │ │ ├ .Adress │ └ .Value │ ├ .Wait │ └ .Time │ └ .End 114 Moving the lift Lift address Position $G, $S 5.11.6.3 1, 2, ∗ work, rinse, shift, special, rest, 0...
5.10 The remote control tree 5.10.8 &Diagnose Objects Description Selection Reference & Root : └ Diagnose ├ .Init │ └ .Select │ │ ├ .RamTest ├ .LcdTest ├ .ContrastTest ├ .KeyTest ├ .IoTest ├ .RsTest ├ .EbusTest ├ .BeeperTest ├ .RackcodeTest ├ .FunctionTest ├ .SimulateKey ├ .InstrNo ├ .OvenTest ├ .Adjust ├ .MeasTest └ .
5 Detailed description 5.11 Description of the remote control commands 5.11.1 &Mode … 116 5.11.1.1 Mode $G, $S, $H, $C Start ($G) or stop ($S) the current method. Interrupt with $H (hold), resume with $C (continue). 5.11.1.2 Mode.Method Name of current method in the working memory. $Q sends 8 ASCII characters. ∗∗∗∗∗∗∗∗ stands for a blank method. 5.11.1.3 Mode.SmplNo 1...999, ∗, Rack Number of samples. This entry determines the number of runs for the sample sequence. ∗ = infinite number of samples.
5.11 Description of the remote control commands 5.11.1.7 Mode.SampleSeq.1.∗ etc. up to .100 .Move…, .Lift…, .Sample…, .Heater…,.Def…, .Flow…, Dos…, Scan…, .Ctrl…, .Wait…, .Rack, .Nop Indexed sample sequence; its commands will be executed line by line in processing. See start sequence (5.11.1.5). 5.11.1.8 Mode.FinalSeq.1.Cmd etc. up to .100 5.11.1.9 Mode.FinalSeq.1.∗ etc. up to .100 5.11.1.10 Mode.Report.
5 Detailed description HTime is the additionally granted waiting time for still reaching the target temperature. HAction is executed after HTime elapses. The SCAN timeout is triggered on execution of a SCAN command. STime determines the reliable response time of the connected device (generally the determination time). SAction is executed after expiry of STime. cont: STOP: ERROR: 5.11.1.13 Mode.Gas.UnitFlow mL/min, L/h Mode.Gas.MinFlow 0…999 Mode.Gas.MaxFlow 0…900…999 Mode.Gas.Select Air, others, N2 Mode.
5.11 Description of the remote control commands 5.11.2 &Config … 5.11.2.1 Config.Aux.Language english, deutsch, français, español Config.Aux.Contrast 0…3…7 Config.Aux.Beeper on, off Config.Aux.DevName 8 ASCII characters Config.Aux.Prog read only Config.Aux.MaxLift 0...90...100 mm Config.Aux.
5 Detailed description 5.11.2.5 Config.RackDef.SpezBeak.1.Pos 0...number of rack positions etc. until .8 Rack positions of special beakers 1 to 8 (position 0 = not defined). 5.11.2.6 Config.PosTab.TabIdx Index of position tables.. 5.11.2.7 Config.PosTab.Name 8 ASCII characters Config.PosTab.R1Num 2...(R2Num – 2) Config.PosTab.R2Num (R1Num + 2)...(R3Num – 2) Config.PosTab.R3Num (R2Num + 2)...200 Config.PosTab.R1Off 0...3599 Config.PosTab.R2Off 0...3599 Config.PosTab.Num 1...
5.11 Description of the remote control commands Configuration of the dosing units. Depending on the selection of the dosing unit (see WetPartNo 5.11.2.9) the corresponding data set is overlayed. These settings are only relevant for Dosinos. For each port of the Dosino individual settings are possible. MaxRate: Max. possible dosing and filling speed allowed Length: Tubing length on selected port Diameter: Inner tubing diameter on selected port 5.11.2.11 Config.RSset $G $G effects all the RS settings.
5 Detailed description 5.11.3 &Info … 122 5.11.3.1 Info.Report $G Info.Report.Select full, short, config, param, usermeth, all $G sends the selected report via RS interface.
5.11 Description of the remote control commands ActHeight: Beaker: Current lift position Beaker exists at tower X (yes/no) 5.11.3.7 Info.ActualInfo.Rack.Code Info.ActualInfo.Rack.Type Info.ActualInfo.Rack.WorkHeight Info.ActualInfo.Rack.RinseHeight Info.ActualInfo.Rack.ShiftHeight Info.ActualInfo.Rack.SpecialHeight Info.ActualInfo.Rack.ActPos Info.ActualInfo.Rack.Act2Pos Current rack data.
5 Detailed description 124 5.11.3.14 Info.ActualInfo.Inputs.Status Status of the Input lines (Input0…7) of the Remote interface. $Q sends the signal state as decimal number e.g. 10 ⇒ 00001010 binary ⇒ 21 + 23 ⇒ Input1 and Input3 active (active = low, inactive = high) See also page 121ff. read only 5.11.3.15 Info.ActualInfo.Outputs.Status read only Status of the output lines (Output0…13) of Remote interface. See 5.11.3.14. 5.11.3.16 Info.ActualInfo.Display.L1 Info.ActualInfo.Display.
5.11 Description of the remote control commands 5.11.4 &Setup … 5.11.4.1 Setup.IdReport Switching on/off the transmission of report identifiers. on, off 5.11.4.2 Setup.Keycode on, off Switching on/off the automatic transmission of keys pressed.
5 Detailed description .Keyboard .Config .Parameter .Usermeth.Recall .UserMeth.Store .Usermeth.Delete .Display 126 Disables all keys of the keyboard, except the , STOP> and key. Locks the configuration menu Locks the parameter menu Locks the function "recall method" Locks the function "store method" Locks the function "delete method" Disables the LCD display. The instrument will not support the display. 5.11.4.6 Setup.Mode.StartWait Indefinite start delay. Only for remote control.
5.11 Description of the remote control commands .Heater.S .E Stop: Switching off of the heater Error: Message with error number (see page 104) Format of AutoInfo messages: (space)!device name"AutoInfo node" Example: !Oven1".G" 5.11.4.10 Setup.PowerOn Simulation of "power on". The method last used is ready for operation. 5.11.4.11 Setup.Initialize Setup.Initialize.
5 Detailed description 5.11.6 &Assembly … 5.11.6.1 Assembly.Sample $G Assembly.Sample.Func =, +, – Assembly.Sample.Value 0...1...999 Defines the (first) sample beaker (rack position) to be processed. Modification of the sample variable. .Func Function .Value Value (absolute or relative) &Assembly.Sample;$G triggers this function. 5.11.6.2 Assembly.Move $G, $S Assembly.Move.Target 1, 2 Assembly.Move.Position sample, spec.1…8, 0...999 Positioning a beaker at the specified tower. .Target Target or tower .
5.11 Description of the remote control commands 5.11.6.7 Assembly.Scan Assembly.Scan.Address Assembly.Scan.Pattern with Rm (parallel/Remote): $G, $S Rm, RS 8 x 1, 0 or ∗ (bin) ready1, end1, Cond ok. Cond 737, no error 14 ASCII characters with RS (serial/RS232): Scanning the interfaces. .Address Selection of interface (Remote / RS232) .Pattern Signal or character string This function is not applicable for process control via RS232 interface. See &Info.ActualInfo.Inputs and …Outputs (5.11.3.14 and 5.11.3.
5 Detailed description 5.11.7 &Diagnosis … 5.11.7.1 Diagnose.Init Diagnose.Init.Select $G param, config, setup, assembly, all RAM initialization. Sets all default values for the selected sub-branch. See also 5.11.4.11. &Diagnose.Init;$G triggers the initialization.. 5.11.7.2 Diagnose.RamTest Diagnose.LcdTest Diagnose.ContrastTest Diagnose.KeyTest Diagnose.IoTest Diagnose.RsTest Diagnose.EbusTest Diagnose.BeeperTest Diagnose.RackcodeTest Diagnose.
5.12 Properties of the RS232 Interface 5.12 Properties of the RS232 Interface 5.12.1 Data Transfer Protocol The 774 Oven Sample Processor is configured as DTE (Data Terminal Equipment). The RS232 interface has the folllowing technical specifications: • Data interface according to the RS232C standard, adjustable transfer parameters, see pages 87 and 145. • Max.
5 Detailed description 774 Oven Sample Processor as Receiver: Sample Changer external device max. 22 characters RxD LF Data output 60 characters Time of 4 characters XOFF XOFF XON TxD Data input String processing 400 µs Time 774 Oven Sample Processor as Sender: Sample changer external device XON XOFF RxD Data output LF TxD Data input Data output max.
5.12 Properties of the RS232 Interface 774 Oven Sample Processor as Sender: Sample Changer external device XOFF Request LF XON RxD Data output 1.Line Response LF LF TxD Data input Data output enabled Data output disabled Time Changer transmission can be stopped by external instruments with XOFF. After XOFF is received the changer completes sending the line already started. If data output is disabled for more than 3 s by XOFF, E43 appears in the display.
5 Detailed description Hardware-Handshake, HWf All handshake inputs are checked, handshake outputs set. 774 Oven Sample Processor as Receiver: Sample Changer external device DTR RxD DTR LF RxD Time 774 Oven Sample Processor as Sender: Sample Changer external device RTS RTS DSR DSR DCD DCD CTS CTS TxD LF TxD Time The data flow can be interrupted by deactivating the CTS line.
5.12 Properties of the RS232 Interface 5.12.3 Pin Assignment RS232C Interface Transmitted Data (TxD). If no data are transmitted, the line is held in the “ON” condition. Data will only be sent when CTS and DSR are in the ”ON” condition and DCD is in the “OFF” condition. Received Data (RxD) Data will only be received when DCD is “ON”. Pin 2 Transmitted Data Pin 3 Received Data Request to Send (RTS) ON condition: the changer is ready to send data.
5 Detailed description Contact arrangement at plug (female) for RS232C socket (male) 13 25 14 1 View of soldered side of plug Order numbers: K.210.9004 and K.210.0001 No liability whatsoever will be accepted for damage or injury caused by improper interconnection of instruments. 5.12.4 What to do if Data Transfer fails? 136 Problem Helpful Questions for Troubleshooting No characters can be received on a connected printer.
6.1 Error messages 6 Appendix 6.1 Error messages If an error occurs, execution of the active command is aborted and an error message is displayed (display blinks). This must be confirmed with the key. If the changer was processing a sample series when the error occurred, it then switches to 'HOLD' state. After the cause of the fault or error has been remedied, the sample series can be continued by pressing key with the next command in the current sequence.
6 Appendix 138 ∗ gas flow too high The gas flow rate is higher than the set max. limit. Regulate the gas flow. ∗ gas flow too low The gas flow rate is lower than the set min. limit. Regulate the gas flow. ∗ gas flow sensor defect The flowmeter is defective. Call your Metrohm servicing technician. ∗ invalid position The selected sample position does not exist or is defined as a special beaker or the selected special beaker is not defined.
6.1 Error messages trap error xxx Unforeseen program error. Switch the unit off and back on again. No display, LEDs light LCD error (system error 7). Inform your servicing technician.
6 Appendix 6.2 Technical data Dimensions Height: 0.51 m, width: 0.38 m, depth: 0.55 m Weight 15.9 kg (not including accessories) Material Sample changer housing: Keypad housing: Metal housing, multiple stove-enamelled Crastin (PBTB), aluminium vapourdeposited on inside Keypad seal: Polyester, resistant to chemicals LCD display 2 lines of 24 characters each, height 5 mm Lift path Approx. 100 mm Lift Load: Lift speed: Turntable Rotary speed: Adjustable, 3...
6.2 Technical data Temperatures Nominal function range 5...40 °C at 20…80 % relative humidity Transportation and storage –20...+60 °C 60 °C relative humidity <50% 50 °C " " <85% 40 °C " " <95% Mains connection Voltage 100...120 V, 220...240 V Frequency 50...60 Hz Power consumption 120 VA Fuses Mains filter: on board 3.774.0110: 2.0 A slow-blow (5 mm ∅, 20 mm in length or 6.3 ∅, 32 mm in length) 0.25 A slow-blow (5 mm ∅, 20 mm in length) All data typical values unless specified otherwise.
6 Appendix 6.3 Maintenance and servicing 6.3.1 Maintenance / service Maintenance of the 774 Oven Sample Processor should be performed within the framework of an annual service carried out by technical personnel of Messrs. Metrohm. If you frequently work with caustic and corrosive chemicals, shorter maintenance intervals will be necessary. The Metrohm Servicing Department offers technical advice on maintenance and servicing of all Metrohm equipment at any time.
6.4 Diagnosis 6.4 Diagnosis 6.4.1 General The 774 Oven Sample Processor is a very precise and reliable unit. Thanks to its rugged construction, its functions can hardly be impaired by external mechanical or electrical influences. Even though the possibility of a fault occurring in the unit can never be entirely precluded, there is a greater possibility of malfunctions occurring as the result of operating errors or incorrect connections and operation with third-party equipment.
6 Appendix 6.4.2 Preparing the instrument • Disconnect the cables to the RS232 and Remote interfaces. • Switch the power on and immediately press key <9> and keep it pressed until the power-up test pattern disappears. LIFT Switch on and 9 drücken. Main menu Diagnosis: diagnosis >RAM initialization diagnosis >RAM test diagnosis >display test Open the sub-menu with Move one menu item down or up with <Ï > or <Ð> Move to the first resp.
6.4 Diagnosis 6.4.3 Main memory (RAM) This diagnosis step completes a non-destructive test of the entire area of the RAM contents (main memory). • Prepare the unit for diagnosis (see Chap. 6.4.2). • If necessary, press <Ð> several times until diagnosis >RAM test • If no errors are found, you will see the following on the display : >RAM test RAM test ok • 6.4.4 Display This diagnosis step allows you to check the LEDs and the display for operability.
6 Appendix 6.4.5 Keypad This diagnosis step allows you to check all keys of the keypad for operability. • Prepare the unit for diagnosis (see Chap. 6.4.2). • If necessary, press <Ð> several times until diagnosis >key test • >key test • Press all keys consecutively and check the response on the display. The corresponding matrix code and designation of the main function for the key pressed are shown on the display (e.g. the following display must be shown when you press key ).
6.4 Diagnosis diagnosis >remote test • >remote test remote test connector ? • Connect the test connector 3.496.8550 to the Remote socket without switching the unit off. • The test runs automatically. If no error occurs, the following is displayed: >remote test remote test ok • Disconnect the test connector and press . 6.4.7 RS232 interface This diagnosis step allows you to check all outputs and inputs for operability. • Prepare the unit for diagnosis (see Chap. 6.4.2).
6 Appendix • If necessary, press <Ð> several times until diagnosis >external bus test • The test searches for all devices connected to the E-Bus interface. The term "devices" means: Tower 1 Dosimat interface (optional, max. 3 ea.) If no error occurs, an identification must be shown on the display for each device connected to the E-Bus. You can scroll through the list of identifications found with key . The following table shows what identifications must be displayed for what configurations.
6.5 Initialise data memory Magnets fitted In this example, the code is: 000110 Magnet fixture viewed from below • Raise the rack and place it to one side. • Prepare the unit for diagnosis (see Chap. 6.4.2). • If necessary, press<Ð> several times until diagnosis >power on reset • The unit runs through the power-up routine (initialisation of lift and rack positions).
6 Appendix Certain device parameters can be set only via RS232, i.e. using a PC. If such device parameters are set and if no PC is available to cancel the settings, the unit cannot be fully set to the previous state. In rare cases, high-magnitude unwanted signals such as mains spikes and lightning strike etc. may impair the contents of the data memory. If the data memory has undefined contents, this may lead to a system crash.
6.5 Initialise data memory • Press key to open the following Diagnosis menu: >RAM initialization select: param 9 >RAM initialization select: config 9 >RAM initialization select: setup 9 >RAM initialization select: assembly >RAM initialization select: all Set method parameters to default values. 9 9 9 9 9 9 © Set device configuration to default values. © Set Setup parameters to default values. © Set Assembly parameters to default values.
6 Appendix 6.6 Validation / GLP GLP (Good Laboratory Practice) demands, amongst other things, a periodic inspection of analytical measuring instruments for reproducibility and correctness on the basis of Standard Operating Procedure (SOPs). Since this unit is not a measuring instrument as such, the user is advised to include the 774 Oven Sample Processor as a part of an analysis system in comprehensive validation of this system.
6.6 Validation / GLP You can use a water standard on an anisole or xylene basis (1.00 mg resp. 0.10 mg water/mL) for validation of a 774 Oven Sample Processor at lower temperatures (<150 °C). The oven temperature must be lower than the boiling point of the solvent used. Recommended settings: Oven temperature: 120 °C Gas flow: Approx. 60 mL/min Sample size: Approx.
6 Appendix 6.7 Warranty and Conformity 6.7.1 Warranty The warranty on our products is limited to defects that are traceable to material, construction or manufacturing error which occur within 12 months from the day of delivery. In this case, the defects will be rectified in our workshops free of charge. Transport costs are to be paid by the customer. For day and night operation, the warranty is limited to 6 months. Glass breakage in the case of electrodes or other parts is not covered by the warranty.
6.7 Warranty and Conformity 6.7.2 EU Declaration of Conformity The Metrohm Ltd. company, Herisau, Switzerland hereby certifies, that the instrument: 774 Oven Sample Processor meets the requirements of EU Directives 89/336/EEC and 73/23/EEC.
6 Appendix 6.7.3 Certificate of Conformity and System Validation 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.
6.8 Accessories 6.8 Accessories 774 Oven Sample Processor includes the following accessories: 2.774.0010 Keyboard Injection needle Outlet needle M6 adapter M6 outer/Luer-Lock Protective cover Plug cover Mains cable with cable socket type CEE(22), V Cable plug to customer's specifications Type SEV 12 (Switzerland...) Type CEE(7), VII (Germany...) Type NEMA/ASA (USA...) Stopper SGJ14 /8 mm FEP tubing M6 44 mm FEP tubing M6 7 mm 2 ea.
6 Appendix Options Accessories to separate order and on payment of extra charge Cables Remote cable 774 — Titrino/756 Coulometer Remote cable 774 — 737 Coulometer RS232 cable 774 — 756 Coulometer 6.2141.020 6.2141.000 6.2125.110 Sample vials Vials 6 mL (Head Space Vials) Septum caps, with aluminium cover and PTFE insert 1000 ea. 1000 ea. 6.2419.000 6.1448.050 Dosing instruments 158 729 Dosimat Interface 2.729.0010 685 Dosimat Mains cable 2.685.0010 6.2134.000 700 Dosino 2.700.
7 Index 7 Index Keys <Í>............................ 30; 46; 47 <9>.........................................144 ................... 35; 48; 60 ................. 23; 45; 63 .............................32; 52 .....................................53 ........................34; 47 ...........48 ...............................31; 51 .....................................46 ................................49 ........................
7 Index diagnosis................................. 142 dialog language ........................ 63 dialog:........................................ 63 diameter .................................... 66 dimensions.............................. 140 display ....................................... 43 display contrast......................... 63 display input signals ................. 52 display locked ........................... 29 DOS ........................................... 79 DOS command ...................
7 Index monitoring the interfaces...........32 MOVE.........................................76 MOVE command .......................76 MOVE function...........................30 move the lift................................30 N needle adapter...........................11 new rack types.........................120 no error ......................................99 normal state ...............................43 number of samples....................68 O object tree ................................
7 Index technical specifications........... 131 temp.correction ......................... 64 temperature control................... 37 temperature profiles .................. 38 temperature range .................. 140 temperature values ................... 70 terminate the sample series...... 35 terminators .............................. 101 text cursor.................................. 60 text editor................................... 60 text entry ....................................
