Metrohm 774 Instructions For Use Manual
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Metrohm 774 Instructions For Use Manual

Oven sample processor
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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
8.774.1043
Instructions for use
Program version 5.774.0010
2005.07 dm

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  • Page 1 CH-9101 Herisau/Switzerland Tel. +41 71 353 85 85 +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 2005.07 dm...

  • Page 3: Table Of Contents

    Table of contents Page Overview Application range___________________________________________ 1 Application possibilities _____________________________________ 1 Instrument description ______________________________________ 3 1.3.1 Oblique view from the right-hand side ......... 3 1.3.2 Oblique view from left-hand side..........4 1.3.3 Rear view..................5 1.3.4 The socket strip (rear panel):............5 1.3.5 Guide head ...................
  • Page 4 Table of contents Page Detailed description 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 Menu organization _________________________________________62 5.3.1 Configuration ................63 5.3.2 Parameters ................. 68 5.3.3 User Defined Methods ...............
  • Page 5 Table of contents Page Appendix Error messages __________________________________________ 137 Technical data____________________________________________ 140 Maintenance and servicing ________________________________ 142 6.3.1 Maintenance / service............... 142 6.3.2 Servicing / care ................. 142 Diagnosis ________________________________________________ 143 6.4.1 General ..................143 6.4.2 Preparing the instrument ............144 6.4.3 Main memory (RAM)..............

  • Page 7: Overview

    After a short familiarization period the operators can alter them to suit their own requirements and store them in the instrument. In this way the 774 Oven Sample Processor can 774 Oven Sample Processor, Instructions for use...
  • Page 8 The standard sample rack offers place for 36 sample vials (22 mm x 38 mm). Freely definable "special beaker" positions can also be defined. These are used for positioning conditioning beakers, which can be selected in each part-sequence, on the rack. 774 Oven Sample Processor, Instructions for use...

  • Page 9: Instrument Description

    Magnetic stirrer Sample rack with 36 places (including condi- tioning position) Oven with protective jacket Plug cover Remote The socket strip: Fuse holder interface Mains switch Mains connection 774 Oven Sample Processor, Instructions for use...

  • Page 10: Oblique View From Left-Hand Side

    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. 774 Oven Sample Processor, Instructions for use...

  • Page 11: Rear View

    External Bus Address RS 232 Keyboard Made by Metrohm Herisau Switzerland External bus Serial connection Keyboard RS 232 interface External bus connection address selector The 'External Bus' address must be set to 0 (zero). 774 Oven Sample Processor, Instructions for use...

  • Page 12: Guide Head

    Guide rod Hollow needle (adjustable) (injection needle) Infrared The tower of the 774 Oven Sample sensors 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.

  • Page 13: Sample Vials

    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 po- sitions on the rack.

  • Page 14: Installation

    Use, page 155). In case of damage see "Warranty", page 154. Setting up The 774 Oven Sample Processor is a rugged instrument and may be used in rough environments such as laboratories and manufacturing plants. It must not be exposed to a corrosive atmosphere.
  • Page 15 (see below). 100 – 120 V 220 – 240 V Power switch Power plug Fuse holder 774 Oven Sample Processor, Instructions for use...

  • Page 16: Safety Considerations

    2 Installation 2.3 Safety considerations • Do not operate the 774 Oven Sample Processor without protective cov- ers. 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.

  • Page 17: Arranging The Accessories

    (for example: a metallic part of the casing of the instru- ment or a radiator) in order to eliminate any static electricity. When peripheral instruments are connected to the 774 Oven Sample Proc- essor, the sample changer and the instruments to be connected have to be switched off, otherwise all instruments could suffer damage.

  • Page 18: Equipping The Guide Head

    2.4.3 Adjusting the sample rack • Check the positioning of the sample rack. After switching on the 774 Oven Sample Processor place the rack on the instrument and let it move to the first sample position by pressing the <...

  • Page 19: Adjusting The Needle Position

    7. Remove rack. Positioning the needle 8. Check the distances according to the draw- ing on the right and adjust if necessary. Distances of the guide head and rod (in mm) 774 Oven Sample Processor, Instructions for use...

  • Page 20: Installation Of The Tubing System And The Drying Flask

    Air supply from the built-in pump A stream of air can be used for the determination of chemically and ther- mally stable samples. The pump built into the tower of the 774 Oven Sam- ple Processor provides a sufficiently large and stable flow rate.

  • Page 21: Installation Of The Measuring Cell

    Metrohm cables. Otherwise safe data transmission may not be guaranteed. Remark: Metrohm cables are labeled with the type of the instrument which they may be connected with and optionally with the particular socket. Look at the ca- ble ends. For example:...

  • Page 22: Remote Connections

    Control of the 756 Coulometer is carried out via the control lines of the re- mote connection. While a sequence is being processed the 774 Oven Sample Processor can, via the serial RS232 interface, cause the 756 Coulometer to load a particu- lar method.
  • Page 23 CTL:Rm : *************1 loads a method in the Coulometer CTL:RS &U.R.N here e.g. "774BLANK" CTL:RS "774BLANK"..$G Scanning the remote lines of the 774: waits for 'cond. ready' SCN:Rm **0**010 waits for end of determination SCN:Rm *****000 774 Oven Sample Processor — 737 Coulometer for coulometric determinations 6.2141.000 cable (remote)
  • Page 24 774 Oven Sample Processor. Please refer to the description of the Metrohm remote language and the 774 remote control tree on page 98ff. 774 Oven Sample Processor, Instructions for use...

  • Page 25: 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.

  • Page 26: Serial Connection (Rs232)

    2.5.3 Serial connection (RS232) Many different instruments may be connected via the serial RS232 inter- face. In addition to all Metrohm instruments that support the Metrohm re- mote 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.

  • Page 27: Connecting A Printer

    Dip SW-2 Dip SW-3 DPU-414 stop bit: parity: none handshake: character set: Seiko The 7-bit ASCII character is set automati- cally to the specific national character set according to the selected dialog lan- guage. 774 Oven Sample Processor, Instructions for use...
  • Page 28 HP Deskjet / 6.2125.020 see printer manual* data bit: Laserjet + serial/ stop bit: with parallel parallel- parity: none * character set PC-8 is required. interface converter handshake: PCL3 command: esc(10U 2.145.0300 character set: 774 Oven Sample Processor, Instructions for use...

  • Page 29: Introduction

    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 de- vices which are connected.

  • Page 30: Oven Settings

    The tower of the 774 Oven Sample Processor is equipped with an infrared- beaker sensor which detects the presence of a sample vial in front of the tower. If the beaker sensor is switched on then this test will be carried out after each MOVE command.

  • Page 31: Rack Definitions

    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 preconfig- ured. Sample position 36 is reserved for a conditioning beaker.

  • Page 32: Dosing Units

    1. In the standard rack for the 774 Oven Sample Processor position 36 is already defined as a special position for the conditioning vessel and should not be altered.

  • Page 33: Rs232 Interface

    PC for controlling the Oven Sample Processor can be connected to the RS232 interface. It is also possible to communicate with other Metrohm instruments (e.g. Coulometer via Metrohm remote control language) and possibly instru- ments from other manufacturers via the interface.

  • Page 34: Lock Keyboard Functions

    '>user methods' + <ENTER> opens the submenu for locking method memory functions. 'lock method recall: on' locks method loading. 'lock method store: on' locks method saving. 'lock method delete: on' locks method deletion. 774 Oven Sample Processor, Instructions for use...
  • Page 35 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. 774 Oven Sample Processor, Instructions for use...

  • Page 36: Manual Operation

    (0 –100 mm), a previously defined posi- tion can be selected with <SELECT> (rest pos = 0 mm, working, rinsing, shift pos, special). Example: LIFT : work <ENTER> LIFT : shift pos <ENTER> LIFT : 50 mm <ENTER> 774 Oven Sample Processor, Instructions for use...
  • Page 37 - Eject the cylinder contents (eject), - Adjust, i.e. remove the play between dosing piston and spindle before aspiration or filling the cylinder (adjust), - Compensate for the play between dosing piston and spindle before dosing (level). 774 Oven Sample Processor, Instructions for use...
  • Page 38 The SCAN function is used for monitoring the serial RS232 and the remote SCAN interfaces. In this way it is possible to check the communication of the 774 Oven Sample Processor with other instruments. The interface can be se- lected with the <SELECT> key and must then be confirmed with <EN- TER>.

  • Page 39: Methods And Sequences

    Final sequence: Command sequence which is carried out once at the end of the series. Course of a method number of samples start sequence final sequence sample sequence <START> normal state 774 Oven Sample Processor, Instructions for use...

  • Page 40: Learn Mode And Trace Function

    • press the <LEARN / HOLD> key • function is stopped, the "LEARN"-LED blinks • use the <ENTER> key to accept the value (or start the LEARN function again) • The "LEARN"-LED goes out, edit the next command line 774 Oven Sample Processor, Instructions for use...

  • Page 41: Process Control

    <STOP> can be used to terminate the sample series completely. If the gas flow limits are exceeded or undercut this does not interrupt the method sequence. The gas flow can be corrected manually with the gas flow regulator. 774 Oven Sample Processor, Instructions for use...

  • Page 42: Power-Up Methods

    774 Oven Sample Processor is switched on and save this method under the name "POWERUP" (see page 75). In the 774 Oven Sample Processor tutorial you will find a list of the exemplary methods stored in the instrument as standard together with comments about them.

  • Page 43: Oven Control And Gas Flow

    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 tempera- ture and transferred to a measuring cell in a stream of carrier gas. The 774 Oven Sample Processor together with the Metrohm Coulometer or a...

  • Page 44: Gas Flow

    774 Oven Sample Processor. However, it is necessary to dry the air with a desiccant such as molecular sieve before it can be used.
  • Page 45 30 mL/min should be set. During needle penetration and removal the gas flow should be switched off as large variations in gas pressure occur during these processes. This avoids unnecessary error messages. 774 Oven Sample Processor, Instructions for use...

  • Page 46: Kf Moisture Determination

    The principle of the oven method with the 774 Oven Sample Processor: Preparation: • The samples are weighed into sample vials and tightly sealed with a PTFE-coated septum.
  • Page 47 The accompanying diagram shows the theoreti- [µg H O/min] cal course of a sample determination with the 774 Oven Sample Processor. It is clear that, in order to determine the amount of water correctly (dark gray area), the blank value must be sub- sample tracted from the total amount of moisture deter- mined.
  • Page 48 Moisture depots lead significant increase of the measured value drift. Reduced reproducibility of results may occur. Please note: The measured value of the Coulometer must not exceed 100 mV. 774 Oven Sample Processor, Instructions for use...

  • Page 49: Detailed Description

    110°C Using key <SELECT/DISPLAY>, you can switch back to measured value display at any time Edit mode Menu title >sample sequence 1 MOVE sample menu line or command second parameter first parameter 774 Oven Sample Processor, Instructions for use...

  • Page 50: The Keyboard

    The lowermost row of keys (<HOLD>, <STOP>, <START>) are used for the direct control of method processing. 774 Oven Sample Processor, Instructions for use...

  • Page 51: Individual Key Functions

    (0 mm), i.e. to the quence can be accessed. upper stop. • Any data that has been altered in a menu or command line is not carried over. See <ENTER> key. 774 Oven Sample Processor, Instructions for use...
  • Page 52 Parame- See <ENTER> key. ter Menu or with the <DEF> key. • The rotation of the rack can only be carried out when the lift is at or above the shift posi- tion. 774 Oven Sample Processor, Instructions for use...
  • Page 53 • The lines following this line are shifted one line downwards. Delete a command line in a sequence DELETE • Deletes the current line in a sequence • The lines which follow shift upwards by one line. 774 Oven Sample Processor, Instructions for use...
  • Page 54 • During processing of a method, the sample series can be aborted with <CLEAR> so that the sam- ple currently being processed is processed to completion. The end sequence is not exe- cuted in this case. 774 Oven Sample Processor, Instructions for use...
  • Page 55 • If a change in a parameter is not confirmed by <ENTER> and another menu line is ac- cessed, the previous value will be reinstated. This is indicated by an acoustic signal. 774 Oven Sample Processor, Instructions for use...
  • Page 56 (work position, shift position, …) in a se- • An absolute lift position in mm quence. can also be given. • An absolute lift position in mm can also be entered. 774 Oven Sample Processor, Instructions for use...
  • Page 57 Dos- ino -’prepare’, ‘release, ‘empty’ and 'release'- can also be executed. • The dosing and filling speed can be set in the parameter menu or with the <DEF> key. 774 Oven Sample Processor, Instructions for use...
  • Page 58 RS 232 inter- or *) for the 14 output lines or face. Use text edit mode. predefined patterns accessi- ble by the <SELECT> key (for ex. "START device1", "STOP instr.1" etc.). 774 Oven Sample Processor, Instructions for use...
  • Page 59 <ENTER> . • The new settings take effect immediately after confirmation of the change by <ENTER>. 774 Oven Sample Processor, Instructions for use...
  • Page 60 • The filling rate may be set individually for every dosing drive (Dosi- mat oder Dosino). • Syntax: FILLRATE [Dosing unit] [Filling speed] FILLRATE Change lift speed • The lift speed can be set at will. • Syntax: LIFTRATE [Tower] [Lift speed] LIFTRATE 774 Oven Sample Processor, Instructions for use...
  • Page 61 • For the second parameter you can choose between the functions: Dosing (Dos), Filling (Fill), Rinsing (Rinse), Empty (Empty) or Pre- pare (Prep). • Syntax: DRIVE.PORT [Dosing drive.Port] [Function] 774 Oven Sample Processor, Instructions for use...
  • Page 62 The rack can be removed in from, ie. the text cursor is the basic position. shifted one place to the right for each instance. See page 60f. 774 Oven Sample Processor, Instructions for use...
  • Page 63 • During a manual halt of a sample series with <STOP>, the end sequence of the method will not be executed. • The manual stop options are also effective in the normal state. 774 Oven Sample Processor, Instructions for use...
  • Page 64 <QUIT> stops a run- ning command and continues with the next command. This is useful when a programmed waiting time is to be shortened or when the expected signal cannot be received during a SCAN command. 774 Oven Sample Processor, Instructions for use...

  • Page 65: Data Entry

    This selection is cyclic, SELECT structured like a revolving drum. Example: >RS232 settings character set: <SELECT> Epson Seiko Citizen <ENTER> >RS232 settings character set: Epson 774 Oven Sample Processor, Instructions for use...

  • Page 66: Text Entry

    Exit text entry With <Quit> text edit mode is exited. The text line displayed can be ac- QUIT cepted with <ENTER> or rejected by pressing <QUIT> a second time. 774 Oven Sample Processor, Instructions for use...
  • Page 67 An entire text line can be entered in this way, for example, for the naming of a method. Text editing can be ended with <QUIT>. The text line will be displayed in its entirety and can be accepted with <ENTER> or rejected with <QUIT>. 774 Oven Sample Processor, Instructions for use...

  • Page 68: Menu Organization

    >RS232 settings <ENTER> either opens a submenu RS control: or confirms data entry at the lower- most menu level. <CONFIG> can be used instead of < >. 774 Oven Sample Processor, Instructions for use...

  • Page 69: Configuration

    This setting of the max. lift path is important as regards safety. Correctly en- tering this value can prevent the puncture needle breaking off since the lift cannot be moved lower than as far as the specified position. 774 Oven Sample Processor, Instructions for use...
  • Page 70 The rack code must be unique and can only occur once in the instrument. >rack definitions Type description of the rack type : M36-0 See p. 88ff. M36-0… <SELECT> enables the choice of Metrohm-specific and self-defined rack types. 774 Oven Sample Processor, Instructions for use...
  • Page 71 Select the dosing unit dosing unit (700 Dosino or 685 Dosimat) 1…12 The address of the dosing unit (see p. 19) must be confirmed with <ENTER>. This will then be displayed in the first menu line. 774 Oven Sample Processor, Instructions for use...
  • Page 72 Parity selection parity: none even, odd, none <QUIT> >RS232 settings Handshake selection to access the handshake: next highest level HWs,HWfull, SWchar,SWline, none >RS232 settings Character set for printer or PC character set: IBM,HP,Epson, Seiko,Citizen 774 Oven Sample Processor, Instructions for use...
  • Page 73 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.

  • Page 74: Parameters

    Up to 99 lines can be entered as a sequence in submenus '>Start Sequence', '>Sample Se- quence' and '>Final Sequence'. The commands can be entered directly on the keyboard. The command keys arranged at the right-hand half of the keyboard are available. 774 Oven Sample Processor, Instructions for use...
  • Page 75 It is automatically occupied by the “NOP” command that has no function. The following lines are shifted one line downwards. <DELETE> deletes the current line in a sequence. The lines following are shifted one line upwards. 774 Oven Sample Processor, Instructions for use...
  • Page 76 Turning speed of the rack in angular shift rate. degrees/second 3…20 >changer settings Turning direction of the rack shift direction: auto. +, -, auto. auto. = the sample changer chooses the shortest path for turning. 774 Oven Sample Processor, Instructions for use...
  • Page 77 A SCAN timeout is triggered if the interface signal is not received immediately when executing a SCAN command. This is normally the case if a connected device is performing a determination and the 774 Oven Sample Processor is to wait for the end of the determination. The SCAN command intercepts the...
  • Page 78 Correction factor for gas flow meas- gas flow factor urement in the case of 'other' gases 0,001…1…9,9 Carrier gas: Factor: Argon 1.456 Methane 0.717 0.738 Natural gas 0.681 Helium 1.456 0.666 Oxygen 0.992 Propane 0.357 774 Oven Sample Processor, Instructions for use...
  • Page 79 >dosing unit Define rinsing inlet (when changing rinsing port dosing units) 1…2…4 >dosing unit Define inlet for the preparation cycle preparation port 1…2…4 >dosing unit Define air inlet for emptying drain port 1…4 774 Oven Sample Processor, Instructions for use...
  • Page 80 The following entries define the commands to be executed when the <STOP> key is pressed. This allows connected peripherals to be stopped automatically or the functions of the 774 Oven Sample Processor to be reset. >manual stop Signal output via remote interface...

  • Page 81: User Defined Methods

    Dialog for deletion of methods >delete method Open the dialog with <ENTER> >delete method Select method method: ******** 8 ASCII characters >delete method Confirm with <ENTER> delete ******** ? Abort with <QUIT> 774 Oven Sample Processor, Instructions for use...

  • Page 82: Command Reference

    The first parameter of this command defines the sample, destination of the rack's MOVE command. Since spec.1…8 the 774 Oven Sample Processor is euipped only 1…999 with Lift 1, it is not practical to enter any other value at this point.
  • Page 83 The first parameter of this command defines the lift rinse, shift, on which the command is to be executed. Since special, rest, the 774 Oven Sample Processor is equipped only 0…100 mm with Lift 1, it is not practical to enter any other value at this point.
  • Page 84 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 Sam- ple Processor. The flow rate is measured and monitored electronically. If the limits set in the methods are overshot or undershot, an error message is displayed.
  • Page 85 Predefined bit patterns are supported which can be selected by short names (for example: "Ready1" or "End1"). "Ready" signifies a static "Ready" line of an external Metrohm instrument. “End" stands for pulse signals, for example EOD (=end of determination). When scanning for pulse signals parallel scanning of several lines cannot be applied.
  • Page 86 (*) is scanned. When it is found, the next part of the character string is compared. This function is especially suited to instruments with Metrohm remote con- trol language. Here the Auto-Info status messages can be scanned. The most useful of these are: *.T.R"...
  • Page 87 Predefined bit patterns are supported which can be selected by short names (for example, "START device1" or "ENTER"). "START device1" starts the operating mode set for a connected Metrohm instrument. "START dosX" starts a Dosimat which is connected to a Metrohm titration instrument via the “activate”...
  • Page 88 5 Detailed description This function is suitable for instruments with Metrohm remote control lan- guage. These can be controlled with so-called triggers. The most important of these are: &M;$G Go, start instrument in current mode &M;$S Stop, stop instrument &M;$H Hold, interrupt method &M;$C...
  • Page 89 The first parameter of this command defines the lift 3…12 mm/s on which the command is to be executed. Since the 774 Oven Sample Processor is equipped only with Lift 1, it is not practical to enter any other value at this point.
  • Page 90 During emptying air will be aspirated via this port. The liquid is ejected via the dosing port. If the dosing device connected is a 685 Dosimat , the port assignments will be ignored. 774 Oven Sample Processor, Instructions for use...

  • Page 91: Printing Reports

    5.5 Printing reports 5.5 Printing reports You can have reports printed out directly by the 774 Oven Sample Proces- sor for documentation purposes. However, this does necessitate connect- ing a printer with serial port to the RS232 socket. This means that no direct RS232 connection to a Metrohm Coulometer 756 is possible.
  • Page 92 1000 mm 2.0 mm 160 mL/min 30 mm 2.0 mm changed values no tube max.rate length diameter >RS232 settings baud rate: 9600 data bit: stop bit: parity: none handshake: character set: RS control: ------------ 774 Oven Sample Processor, Instructions for use...
  • Page 93 100 mL/min gas type: >dosing unit def. Behaviour in the event of manual method abort >manual stop CTL Rmt: ************** CTL RS232: FLOW: HEATER: INIT °C ------------ See the Tutorial for further method listings. 774 Oven Sample Processor, Instructions for use...

  • Page 94: Automatic Reports

    Manual reports can also be output at the press of a key. In order to do this, press key <PRINT> and choose the required report with <SELECT>. The 'full' and 'short' reports each contain the data of the last sequence run. 774 Oven Sample Processor, Instructions for use...

  • Page 95: 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 de- tached to insert samples and can then be fitted back on again. It is de- signed for 35 sample vials whose dimensions must correspond to the specifications so that these vials (22 mm Head Space Vials, order No.
  • Page 96 (0-3599) of the full turning angle. The rack type is coded as Mxx-y, whereby M stands for Metrohm-defined types. The placeholder xx stands for the number of sample beakers in a rack. The numerical code y is reserved for special racks (unused as yet).
  • Page 97 If a special beaker is required in a method process but the changer finds no vial present in the reserved position, an error message will always be dis- played. 774 Oven Sample Processor, Instructions for use...

  • Page 98: Dosimats And Dosinos

    The changer automatically recognizes the type of the connected dosing in- strument. Further commands are available for the 700 Dosino so that the many and varied abilities of these dosing units can be fully taken advantage of. 700 Dosino 700 Dosino 10 ml 774 Oven Sample Processor, Instruction for use...
  • Page 99 – is situated on the side and not defined in standard operation. Port 4 – is situated on the bottom and during standard operation is defined as an air inlet when emptying the tubing systems. 774 Oven Sample Processor, Instruction for use...
  • Page 100 During preparation, the burette as well as the filling and dosing tubing are completely filled. Several filling and dosing processes are executed for this. The volumes required for this are internally 774 Oven Sample Processor, Instruction for use...
  • Page 101 To fill the burette for example, with distilled water for storage, this can be changed with the following commands. >dosing unit def. rinsing Port Y <DEF> DRIVE.PORT XX.Y : rinse 774 Oven Sample Processor, Instruction for use...
  • Page 102 The mechanical play between the dosing piston and the spindle is com- pensated after the cock has been turned into the dosing position. The dosing port can be redefined as desired (see Dosing). This command is executed to increase the precision. 774 Oven Sample Processor, Instruction for use...

  • Page 103: Remote Interface

    Pin 20 Various remote cables are available to use the specific functions of the indi- vidual instruments of the various Metrohm model lines (see page 16ff). Metrohm also delivers special cables on request suited to the customer’s needs, which allow complex couplings (including foreign instruments).
  • Page 104 (∗). To simplify the use of these remote control commands especially when connecting several instruments with Metrohm cables, the following com- mand parameters are available for the CTL and SCN commands. See next page.
  • Page 105 (EOD) ****1*** Cond ok queries "Cond" state of device1 (Titrinos. …) ******1* Cond 737 queries "Cond" state of the 737 Coulometer 1****1** no error queries "no error" state of device1 (Titrinos. …) **1***** 774 Oven Sample Processor, Instructions for use...
  • Page 106 5 Detailed description 774 Oven Sample Processor, Instructions for use...

  • Page 107: 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.

  • Page 108: Calling Up Objects

    'Language' at this level: ..L wards require n+1 preceding dots. Change from node 'Language' via the root to If you must jump back to the root, enter a pre- node 'Mode': &M ceding &. 774 Oven Sample Processor, Instructions for use...

  • Page 109: Triggers

    The instrument has been restarted actively after hold. Ready The instrument has executed the last command and is ready. Stop A process has been aborted, e.g. by pressing the <STOP> key or because there was an error. 774 Oven Sample Processor, Instructions for use...

  • Page 110: Error Messages, Errors

    Stop bit error Exit: <QUIT>and set the same stop bit for both instruments. Overrun error. At least 1 character could not be read. Exit: <QUIT>. Internal receive buffer full (>82 characters). Exit: <QUIT>. 774 Oven Sample Processor, Instructions for use...
  • Page 111 Gas flow too low E165 Max. temperature reached E168 Temperature sensor defect E169 Flowmeter defect E201 Changer function error (div.) E202 Dosimat function error E206 Gas flow too high E207 Error list full E208 SCAN timeout 774 Oven Sample Processor, Instructions for use...

  • Page 112: The Remote Control Tree

    │ │ ├ .Cmd Command nop, MOVE, LIFT, 5.11.1.7 ∗ │ │ └ SAMPLE, HEATER, DEF │ │ FLOW, DOS, SCAN, ∗ │ CTRL, WAIT, RACK │ : │ └ .100 Sequence end │ 774 Oven Sample Processor, Instructions for use...
  • Page 113 STOP device1, 5.11.1.15 │ 14 x 1, 0 or ∗ (bin) ├ .RSCtl Command via RS232 &M;$S, 14 ASCII characters ├ .FLOW Gas flow control cont., off └ .HEATER Heater control INIT, off, 50…250 774 Oven Sample Processor, Instructions for use...

  • Page 114: Config

    Number of positions 1...200 │ ├ Position 1 │ │ └ .Value Position in 1/10-ang. degr. 0...3599 │ : │ └ .12, 14, 16, 24, 48, i.e. PosTab.Num └ .Value Position in -angular degr. 0...3599 774 Oven Sample Processor, Instructions for use...

  • Page 115: Info

    │ usermeth, all │ └ .DetermData Determination data 5.11.3.2 ├ .Mplist Meas. point list of temperature : ├ Meas. point 1 : └ Temperature in °C read only └ .400 Meas. point 400 774 Oven Sample Processor, Instructions for use...
  • Page 116 │ ├ .Pump Pump 5.11.3.9 │ └ .State State read only │ ├ .OutHeater Outlet heater 5.11.3.10 │ └ .State State read only │ ├ .Fan 5.11.3.11 │ └ .State State read only 774 Oven Sample Processor, Instructions for use...
  • Page 117 Text line 1 read only │ └ Text line 2 read only │ └ .Counter Sample counter 5.11.3.17 ├ .Sample Current sample position read only └ .Maximum Number of samples to process read only 774 Oven Sample Processor, Instructions for use...

  • Page 118: Setup

    │ │ ├ Begin of method on, off │ │ ├ End of process on, off │ │ ├ Begin start sequence "OMove" on, off │ │ └ End final sequence "CMove" on, off 774 Oven Sample Processor, Instructions for use...

  • Page 119: Usermeth

    =, +, – │ └ .Value Value of function 0...1...999 │ ├ .Move Turning the rack $G, $S 5.11.6.2 │ ├ .Target Lift selection 1, 2 │ └ .Position Beaker or position sample, spec.1...8, 1...999 774 Oven Sample Processor, Instructions for use...
  • Page 120 │ └ .Value Value dependent upon item │ ├ .Wait Waiting time $G, $S, $H, $C 5.11.6.10 │ └ .Time Waiting time 0...1...9999 s │ └ .End Changer RACK / RESET 5.11.6.11 774 Oven Sample Processor, Instructions for use...

  • Page 121: Diagnose

    Instrument number (Not accessible via RS232) 5.11.7.4 ├ .OvenTest Test heater $G, $S 5.11.7.5 ├ .Adjust Temperature meas. adjustment $G, $S ├ .MeasTest Test temperature measurement $G, $S └ .PowerOn Power-on simulation 5.11.7.6 774 Oven Sample Processor, Instructions for use...

  • Page 122: Description Of The Remote Control Commands

    Mode.SampleSeq.1.Cmd NOP, MOVE, LIFT, SAMPLE, etc. up to .100 HEATER, DEF, FLOW, DOS, SCAN, CTRL, WAIT, RACK Defines the command of the indexed command line in a sample sequence. See start sequence (5.11.1.5). 774 Oven Sample Processor, Instructions for use...
  • Page 123 Timeout settings. Timeout times are defined in seconds. The HEATER timeout occurs if the set oven temperature (in the case of the HEATER command) is not reached after the specified heating (in minutes). 774 Oven Sample Processor, Instructions for use...
  • Page 124 The pump and the solenoid valve remain in the current state or are both deactivated .HEATER Oven control is either set to the initial temperature or switched off. Any temperature may also be selected 774 Oven Sample Processor, Instructions for use...

  • Page 125: Config

    Rinsing position of the lift in mm from the upper stop of the tower. ShiftH: Shifting position of the lift in mm from the upper stop of the tower. SpecialH: Special position of the lift in mm from the upper stop of the tower. 774 Oven Sample Processor, Instructions for use...
  • Page 126 • Enter the particular angular offset for each rack position (Irregular layouts of rack positions are possible) 5.11.2.9 Config.WetPart.WetPartNo 1...12 Identification of dosing unit. 5.11.2.10 Config.WetPart.1.MaxRate 0.01...160 ml/min Config.WetPart.1.Length 0...1000...30000 mm Config.WetPart.1.Diameter 0.1...2...20 mm until .4.Diameter (Default value .2.Length : 250 mm) 774 Oven Sample Processor, Instructions for use...
  • Page 127 131ff. 5.11.2.13 Config.RSset.CharSet IBM, HP, Epson, Seiko, Citizen Setting the character set and print mode. For data communication with computers select 'IBM' (IBM code page 437). 774 Oven Sample Processor, Instructions for use...

  • Page 128: Info

    Info.ActualInfo.Lift.1.ActHeight read only Info.ActualInfo.Lift.1.Beaker read only Info.ActualInfo.Lift.2.Exist read only Info.ActualInfo.Lift.2.MaxHeight read only Info.ActualInfo.Lift.2.ActHeight read only Info.ActualInfo.Lift.2.Beaker read only Current data of lift 1 and 2. Exist: Tower exists (yes/no) MaxHeight: Preset max. height 774 Oven Sample Processor, Instructions for use...
  • Page 129 Info.ActualInfo.Buret.1.Volume read only etc. until .12 Current data of dosing drive. State: Status (ready/busy) Position: Piston position in mL Cock: Cock position Type: Type of dosing unit (685/700) Volume: Burette volume 774 Oven Sample Processor, Instructions for use...
  • Page 130 Info.ActualInfo.Display.L1 read only Info.ActualInfo.Display.L2 read only Text of the first and second line of the LCD display. 5.11.3.17 Info.ActualInfo.Counter.Sample read only Info.ActualInfo.Counter.Maximum read only Currently processed sample number and total number of samples. 774 Oven Sample Processor, Instructions for use...

  • Page 131: Setup

    The beginning of the message is marked with a space (ASCII 32). 5.11.4.5 Setup.Lock.Keyboard on, off Setup.Lock.Config on, off Setup.Lock.Parameter on, off Setup.Lock.UserMeth.Recall on, off Setup.Lock.UserMeth.Store on, off Setup.Lock.UserMeth.Delete on, off Setup.Lock.Display on, off "on" means disable the corresponding function. 774 Oven Sample Processor, Instructions for use...
  • Page 132 Continue: Resuming after Hold .Ch.B Begin: Begin of sample sequence .Ch.F Final: End of sample sequence .Ch.OM "Opening Moves": Begin of start sequence .Ch.CM "Closing Moves": Begin of final sequence .Heater.T Target: Change of target temperatur 774 Oven Sample Processor, Instructions for use...

  • Page 133: Usermeth

    .DelAll;$G deletes all method in the user memory. 5.11.5.3 UserMeth.List.1.Name read only UserMeth.List.Bytes read only for each method List of all method in the user method memory including method name and file size in bytes. 774 Oven Sample Processor, Instructions for use...

  • Page 134: Assembly

    Assembly.Dos $G, $S Assembly.Dos.Address 1...12 Assembly.Dos.Value ±0.01…999.999 ml, fill, release, prepar., empty , eject, adjust, level Control of dosing units. .Address Selection of dosing unit .Value Volume or function &Assembly.Dos;$G triggers this function. 774 Oven Sample Processor, Instructions for use...
  • Page 135 &Assembly.Def;$G triggers this function. 5.11.6.10 Assembly.Wait $G, $S, $H, $C Assembly.Wait.Time 0...1...9999 s Waiting time. &Assembly.Wait;$G triggers this function. 5.11.6.11 Assembly.End $G triggers a RESET (same as the <RACK> key). 774 Oven Sample Processor, Instructions for use...

  • Page 136: Diagnosis

    Instrument number. This entry is not accessible via RS232 interface. 5.11.7.5 Diagnose.OvenTest $G, $S Diagnose.Adjust $G, $S Diagnose.MeasTest $G, $S .OvenTest Heater test. .Adjust Adjustment of temperature and gas flow measurement. .MeasTest Test of temperature measurement. 5.11.7.6 Diagnose.PowerOn Simulation of 'Power on'. 774 Oven Sample Processor, Instructions for use...

  • Page 137: Properties Of The Rs232 Interface

    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.
  • Page 138 Afterwards the changer sends XON and is again ready for receiving. 774 Oven Sample Processor as Receiver: Sample Changer external device Input disabled Data output XOFF Data input String 400 µs processing Time 774 Oven Sample Processor, Instructions for use...
  • Page 139 774 Oven Sample Processor as Receiver: Sample Changer external device Time 774 Oven Sample Processor as Sender: Sample Changer external device Time The data flow can be interrupted by deactivating the CTS line. 774 Oven Sample Processor, Instructions for use...
  • Page 140 774 Oven Sample Processor as Receiver: Sample Changer external device Time 774 Oven Sample Processor as Sender: Sample Changer external device Time The data flow can be interrupted by deactivating the CTS line. 774 Oven Sample Processor, Instructions for use...

  • Page 141: Pin Assignment

    (<–3 V): OFF state voltage positive (>+3 V): ON state In the transitional range from +3 V to –3 V the signal state is undefined. Driver 14C88 according to EIA RS232C specification Receiver 14C89 " " 774 Oven Sample Processor, Instructions for use...

  • Page 142: What To Do If Data Transfer Fails

    − Is the baud rate set the same on both devices? garbled. − Is the correct printer selected? − The data transmission was interrupted (by the hardware) during printing. Re-establish connections again, turn printer off and on. 774 Oven Sample Processor, Instructions for use...

  • Page 143: Appendix

    Check the burette and plunger. More than 10 error messages have occurred. Check the unit. ∗ error list full Switch the unit off and back again if necessary. Restart the sample series. 774 Oven Sample Processor, Instructions for use...
  • Page 144 The gas flow rate is lower than the set min. limit. Regulate ∗ gas flow too low the gas flow. The flowmeter is defective. Call your Metrohm servicing tech- ∗ gas flow sensor defect nician. The selected sample position does not exist or is defined as ∗...
  • Page 145 6.1 Error messages Unforeseen program error. Switch the unit off and back on trap error xxx again. LCD error (system error 7). Inform your servicing No display, LEDs light technician. 774 Oven Sample Processor, Instructions for use...

  • Page 146: Technical Data

    Input: >20 ms active = low inactive = high Output: >200 ms = 40 V active = low = 20 mA inactive = high +5 V: maximum load = 20 mA 774 Oven Sample Processor, Instructions for use...
  • Page 147 EN 50081-1/2 1992, EN 55011 (Class B), EN 55022 (Class B) and NAMUR. Interference immunity Standards EN 50082-1/2 1997/1995, IEC 801-2 to IEC 801-6, 61000-3-2/1995, 61000-3-3/1995 and 61000-4-11 are complied with. Emitted interference Laboratory Apparatus Standard IEC61326-1/1997 and interference immunity 774 Oven Sample Processor, Instructions for use...

  • Page 148: Maintenance And Servicing

    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.

  • Page 149: Diagnosis

    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 en-...

  • Page 150: Preparing The Instrument

    >beeper test diagnosis >rack code test diagnosis >function test diagnosis >instrument number diagnosis >oven test diagnosis >instrument adjustment diagnosis >measure test diagnosis power on reset * These tests are reserved for servicing personnel. 774 Oven Sample Processor, Instructions for use...

  • Page 151: Main Memory (Ram)

    After you press the <ENTER> key, the following display is shown, whereby the contrast of the display is varied constantly between bright and dark. >display contrast test 774 Oven Sample Proc. • The test can be quit with key <QUIT> or <STOP>. 774 Oven Sample Processor, Instructions for use...

  • Page 152: Keypad

    This diagnosis step allows you to check all outputs (14) and inputs (8) for operability. • Prepare the unit for diagnosis (see Chap. 6.4.2). • If necessary, press < > several times until 774 Oven Sample Processor, Instructions for use...

  • Page 153: Rs232 Interface

    • Disconnect the test connector and press <ENTER>. 6.4.8 External bus interface This diagnosis step allows you to check all parts of the external bus inter- face for operability. • Prepare the unit for diagnosis (see Chap. 6.4.2). 774 Oven Sample Processor, Instructions for use...

  • Page 154: Beeper

    • Note down the coding (magnets) on the underside of the racks for all racks used for the test. The magnet fixture on the underside of the rack is shown in the diagram below. 774 Oven Sample Processor, Instructions for use...

  • Page 155: Initialise Data Memory

    This diagnosis step allows you to assign default values to device parame- ters using the keypad and thus set the unit to its original state. This is im- portant owing to the following two aspects: 774 Oven Sample Processor, Instructions for use...
  • Page 156 If the data memory has undefined contents, this may lead to a system crash. The 774 Oven Sample Processor offers various options for initialising the data memory. Either the entire memory ( ) or only parts of it (param, ) may be assigned default values.
  • Page 157 • If necessary, press key <Select> several times until: >RAM initialization select: • Press <ENTER>. diagnosis >RAM test • Press <QUIT>. The Diagnosis menu is closed and the device runs through a power-up reset. 774 Oven Sample Processor, Instructions for use...

  • Page 158: Validation / Glp

    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.
  • Page 159 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 boil- ing point of the solvent used.

  • Page 160: Warranty And Conformity

    Metrohm from any liability to pay compen- sation. If any instruments and parts have to be returned, the original packaging should be used if at all possible.

  • Page 161: Eu Declaration Of Conformity

    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. Source of specifications: EN 50081 Electromagnetic compatibility, basic specification Emitted Interference...

  • Page 162: Certificate Of Conformity And System Validation

    The features of the system software are documented in the instruction manual. Metrohm Ltd. is holder of the SQS certificate of the quality system ISO 9001 for quality assurance in design/development, production, installation and servicing.

  • Page 163: Accessories

    1000 ea. 6.2419.000 Aluminum crimp seals/septa with PTFE insert 1000 ea. 6.1448.050 Instructions for use for 774 Oven Sample Processor 8.774.1043 Quick reference for 774 Oven Sample Processor 8.774.1011 Tutorial for 774 Oven Sample Processor 8.774.1021 774 Oven Sample Processor, Instructions for use...
  • Page 164 Vials 6 mL (Head Space Vials) 1000 ea. 6.2419.000 Septum caps, 1000 ea. 6.1448.050 with aluminium cover and PTFE insert Dosing instruments 729 Dosimat Interface 2.729.0010 685 Dosimat 2.685.0010 Mains cable 6.2134.000 700 Dosino 2.700.0010 774 Oven Sample Processor, Instructions for use...

  • Page 165: Index

    40 delete lines ........ 34 blank value......... 41 delete method ......75 built-in pump......12 detailed description....43 burette........92 device label ....... 63 burette size ........ 66 device-specific errors....105 774 Oven Sample Processor, Instructions for use...
  • Page 166 103 methods ........33 filling the cylinder....... 31 instrument label......63 min. flow........72 FILLRATE......54; 83 instrument status ...... 43 missing beaker ......71 final sequence ......33 integration ......... 15 molecular sieve......14 774 Oven Sample Processor, Instructions for use...
  • Page 167 43 printer emulations ......21 sample determination....41 printing reports ......85 SAMPLE function....... 31 target temperature..... 51 process control......35 sample preparation ....40 technical data ......140 program ........63 sample rack .....6; 13; 89 774 Oven Sample Processor, Instructions for use...
  • Page 168 TRACE function ....35; 57 upwards ........30 tracing........57 user defined methods....75 tracing a method ....... 35 user method menu....45 zero-position ......45 transmission speed....66 user method report ....85 transmit........32 774 Oven Sample Processor, Instructions for use...

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