Metrohm 711 User Manual

711 Liquino

Manual

8.711.1023

Metrohm AG CH-9101 Herisau Switzerland Phone +41 71 353 85 85 Fax +41 71 353 89 01 info@metrohm.com www.metrohm.com

711 Liquino

Manual

8.711.1023 02.99 dm

Teachware Metrohm AG CH-9101 Herisau teachware@metrohm.com

Although all the information given in this documentation has been checked with great care, errors cannot be entirely excluded. Should you notice any mistakes please send us your comments using the address given above.

Documentation in additional languages can be found on

http://products.metrohm.com under Literature/Technical documenta-

tion.

Table of content

page

1 Overview 1

1.1 Application range __________________________________________1

1.2 Application possibilities ____________________________________1

1.3 Instrument description ______________________________________2

1.3.1 Front view ......................................................................................... 2

1.3.2 Rear view .......................................................................................... 3

2 Installation 4

2.1 Instrument setup __________________________________________4

2.1.1 Mains connection ............................................................................. 4

2.2 Safety information _________________________________________5

2.3 Setup ____________________________________________________7

2.3.1 Connecting the keyboard ................................................................. 7

2.3.2 Connecting the Dosinos ................................................................... 7

2.3.3 Connecting a Pt100 temperature sensor ......................................... 7

2.3.4 Installing the pipetting attachment ................................................... 8

2.4 Memory card ______________________________________________8

2.5 Connections ______________________________________________9

2.5.1 Remote connections ...................................................................... 10

2.5.2 Serial connections .......................................................................... 16

2.5.3 Connecting a printer ....................................................................... 17

2.5.4 Connecting a balance .................................................................... 19

3 Introduction 20

3.1 The Liquino concept ______________________________________20

3.2 Tutorial _________________________________________________21

3.2.1 Basic configuration ......................................................................... 21

3.2.2 Defining dosing units ...................................................................... 22

3.2.3 Dosing and dispensing .................................................................. 24

3.2.4 Changing the dosing unit ............................................................... 28

3.2.5 Temperature measurement ............................................................ 29

3.2.6 PIP – precise pipetting/diluting ....................................................... 30

3.2.7 SMPL – fully automatic sampling ................................................... 33

3.2.8 CONT – the automatic volumetric flask .......................................... 40

3.2.9 XDOS – the electronic dropping funnel .......................................... 43

3.2.10 XDOS – temperature-controlled addition ..................................... 46

3.2.11 SEQ – complex procedures under control ................................... 51

3.2.12 GLP – automatic validation ........................................................... 57

4 Detailed description 61

4.1 The keyboard ____________________________________________61

4.1.1 Menu keys ...................................................................................... 62

4.1.2 Action keys ..................................................................................... 62

4.1.3 Editing and navigating keys ........................................................... 62

4.1.4 Manual functions and other keys ................................................... 63

4.2 Editing __________________________________________________65

4.2.1 Navigating in menus ....................................................................... 65

4.2.2 Data input ....................................................................................... 65

4.2.3 Text input ........................................................................................ 66

4.3 Configuration ____________________________________________68

4.3.1 Defining the dosing units ................................................................ 68

4.3.2 The configuration menu .................................................................. 69

4.3.3 Keyboard and graphics options ..................................................... 71

711 Liquino, Instructions for use

Table of content

page

4.4 XDOS mode - controlled dosing ____________________________ 74

4.4.1 XDOS mode parameters ................................................................ 77

4.4.2 Examples of reports - XDOS mode ................................................ 81

4.5 SEQ mode - complex processes ____________________________ 83

4.5.1 Commands ..................................................................................... 84

4.5.2 SEQ mode parameters .................................................................. 89

4.5.3 Commands in a sequence ............................................................. 91

4.5.4 Example of a report - SEQ mode ................................................... 93

4.6 CONT mode - preparation of solutions ______________________ 94

4.6.1 Preparation of solutions ................................................................. 94

4.6.2 Standard solutions / Dilutions ........................................................ 95

4.6.3 CONT mode parameters ................................................................ 96

4.6.4 Example of a report - CONT mode ................................................ 99

4.7 PIP mode - precise pipetting and diluting ___________________ 100

4.7.1 PIP mode parameters .................................................................. 103

4.7.2 Example of a report - PIP mode ................................................... 105

4.8 SMPL mode - fully automatic sampling _____________________ 106

4.8.1 Sampling process in detail ........................................................... 110

4.8.2 SMPL mode parameters .............................................................. 113

4.8.3 Example of report - SMPL mode .................................................. 118

4.9 GLP mode - validation ___________________________________ 120

4.9.1 GLP mode parameters ................................................................. 123

4.9.2 Example of report - GLP mode .................................................... 125

4.10 Storing and loading methods ____________________________ 128

4.10.1 Internal method memory ............................................................ 128

4.10.2 Memory card .............................................................................. 129

5 The 711 Liquino in synthesis laboratories 133

5.1 The advantages of the 711 Liquino _________________________ 133

5.2 Please note … __________________________________________ 135

6 Appendix 139

6.1 Dosing units and Dosinos ________________________________ 139

6.1.1 Preparing and emptying the dosing units .................................... 141

6.1.2 Defining dosing units ................................................................... 143

6.2 Error messages _________________________________________ 144

6.3 Service and maintenance _________________________________ 148

6.3.1 Service .......................................................................................... 148

6.3.2 Maintenance / Care ...................................................................... 148

6.4 Validation / GLP ________________________________________ 149

6.5 Diagnosis ______________________________________________ 150

6.6 Initialize data memory ___________________________________ 160

6.7 Technical specifications _________________________________ 162

6.8 Warranty and certificates _________________________________ 164

6.8.1 Warranty ....................................................................................... 164

6.9 EC Declaration of conformity _____________________________ 165

6.9.1 Certificate of Conformity and System Validation .......................... 166

6.10 Accessories ___________________________________________ 167

7 Index 171

711 Liquino, Instructions for use

1. Overview

1

1 Overview

1.1 Application range

The Metrohm 711 Liquino is a very versatile laboratory instrument which can be used everywhere that liquid handling is to be simplified and automated. This is the case in both analytical laboratories and in synthesis laboratories. It is equally suitable for both the preparation of complicated formulations in filling plants and also for simple delivery and pumping tasks involving toxic or aggressive media. Owing to the freely programmable process sequences and versatile communication interfaces (RS232 or remote connection) it can be integrated into complex automated systems to undertake demanding dosing and monitoring functions, which otherwise would only be capable of realization with a considerably greater expenditure.

1.2 Application possibilities

The 711 Liquino can be used for the whole range of applications which fall under the general heading of 'Liquid Handling'.

In analytical laboratories

• manual, highly accurate liquid dosing.

• complex, process-controlled dosing tasks with freely selectable specifi-

cations, e.g. a certain volume in a given period, constant dosing speed during a preselected time interval, a certain volume with constant dosing speed. In addition this can also be temperature-controlled, i.e. if a certain temperature limit is exceeded or undercut during the dosing process then the dosing process can be interrupted and a predefined action triggered, e.g. switching on a cooling bath.

• automated preparation of defined solutions (e.g. standard solutions) or

mixtures of liquids (e.g. mobile phases for HPLC or IC). It is possible to connect a balance without any problems.

• highly accurate pipetting and diluting even small volumes of liquid.

• automated sampling and sample preparation for a range of analytical

methods (e.g. titrations, pH measurements, etc.) with and without a sample changer.

• preparation of complex formulations in automated filling plant.

In synthesis laboratories

• manual, highly accurate liquid dosing.

• complex, process-controlled dosing tasks with freely selectable specifi-

cations, e.g. a certain volume in a given period, constant dosing speed during a preselected time interval, a certain volume with constant dosing speed. In addition this can also be temperature-controlled, i.e. if a certain temperature limit is exceeded or undercut during the dosing process then the dosing process can be interrupted and a predefined action triggered, e.g. switching on a cooling bath.

711 Liquino, Instructions for use

1.3 Instrument description

2

Slot for memory

Always insert the card so that

1.3 Instrument description

1.3.1 Front view

card

the upper edge of the card with the label faces right.

711 Liquino, Instructions for use

1. Overview

3

- Fire Hazard For continued pr ot ection replace only with the same type and rating of fuse

Fuse:

100/115V : 315mAT 230/240V : 160mAT

Keyboard/Display

Rem ot e

RS 232

Pt 100

Dos.4

Dos.3

Dos.2

Dos.1

Made by Metrohm Herisau Switzerland

WARNING !

Connections for

Connection for

Keyboard connection

Remote

Serial RS 232

Fuses, mains switch

Name plate

1.3.2 Rear view

4 Dosinos

Pt100 temperature sensor

interface

and mains connection

711 Liquino, Instructions for use

2.1 Instrument setup

4

Follow the ins supply. If the instrument is operated with the mains voltage incorrectly set and/or the wrong mains fuse there may be a fire risk!

2 Installation

2.1 Instrument setup

Packaging

The 711 Liquino is supplied in packaging which provides excellent protection. This includes a shock-absorbing plastic foam lining. Please store this packaging as it is the only way to guarantee damage-free transport of the instrument.

Checks Please check immediately on receipt whether the shipment is complete and undamaged.

Location The 711 Liquino is a robust instrument and can therefore be used even under rough conditions in laboratories and factories. However, care must be taken that it is not exposed to a corrosive atmosphere. Regular care of the instrument is essential if it is used in rough surroundings.

2.1.1 Mains connection

Setting the mains supply

Before switching on the 711 Liquino for the first time check that the mains voltage set on the instrument (see illustration on following page) corresponds to the local mains voltage. If this is not the case then the correct mains voltage must be set as follows:

• Pull out mains cable

Remove the mains cable from the mains connector of the 711 Liquino.

• Remove fuse holder

Use a screwdriver to loosen the fuse holder beside the mains connector and remove completely.

• Check and replace fuses

Remove the built-in fuses for the required mains voltage from the fuse holder and check their specifications:

100…120 V 0.315 A (slow-blow) Metrohm no. U.600.0011 220…240 V 0.16 A (slow-blow) Metrohm no. U.600.0008

tructions given below to connect the instrument to the mains

• Insert fuses

Exchange fuses if necessary and replace them in the fuse holder.

• Set mains voltage

Remove the white fuse block from the fuse holder and reinsert it so that the correct mains voltage is visible through the window in the fuse holder.

711 Liquino, Instructions for use

2. Installation

5

230

Mains switch

Mains connection socket

Fuse holder with window

• Insert fuse holder

Insert fuse holder and press it until it clicks into place.

2.2 Safety information

General This instrument left our factory in perfect condition from a safety point of view. The following information must be carefully observed in order to maintain this condition and to ensure hazard-free operation.

Mains connection The mains cables supplied with the instrument are three-core and are fitted with an earthing pin. If a different plug must be used then the yellow/green lead must be connected to the protective earth.

WARNING!

Any break in the earth conductor inside or outside the instrument can represent a source of danger to the operator. Making a break in the earth conductor is forbidden.

Before connecting the plug to the mains supply a check must be made that the instrument is set to the local mains voltage and that the appropriate fuses are inserted.

WARNING!

When changing a fuse and when setting a different mains voltage the mains cable must be disconnected from the mains supply.

When replacing fuses care must be taken that voltage, current and type have been selected correctly (see Technical data, fuses, page 162).

WARNING!

Short-circuiting fuses or the temporary use of incorrect fuses is forbidden.

Repair and maintenance:

If faults or malfunctions occur during the operation of the 711 Liquino it is recommended that the cable connections with the peripheral units are checked first for proper functioning (see page 9ff). It may be possible to lo-

711 Liquino, Instructions for use

2.2 Safety information

6

out.

cate the source of the fault with the aid of the diagnosis functions. If the cause of the malfunction cannot be found please contact the Metrohm service department.

The instrument should only be opened when switched on under exceptional circumstances. As this exposes electrically live components it should only be carried out by an expert who is familiar with the risks involved.

The instrument must be separated from all electricity sources before it is opened. Make sure that the mains plug has been pulled

Condensers in the instrument may still be charged even when the instrument is no longer connected to the mains supply.

Changing the battery The connecting wires of the old battery must be cut before desoldering so that any residual charge which may still be present cannot be shortcircuited. The polarity of the new battery must be taken into account when it is fitted. Lithium batteries cannot be recharged and should not be short-circuited or exposed to temperatures above 70 °C under any circumstances. Old batteries must be disposed of in an environmentally acceptable way and must not be burnt.

Static electricity: The circuit contains components which could be destroyed by electrostatic charges or whose functions could be affected by them. Work on an open instrument should only be carried out in ESD-protected surroundings.

Suitable measures:

1. A conductive mat on the work surface connected to the earth conductor

via a resistor of approx. 1 MΩ.

2. Earthed soldering iron.

3. Persons working with components must have their wrists connected to

the earth conductor via a resistor of approx. 1 MΩ.

4. Components and assembled PCBs should only be stored and transported in conductive packaging or foam.

5. New components should be stored in their original packaging until re- quired.

If it becomes apparent that the instrument can no longer be operated safely then it should not be used at all.

711 Liquino, Instructions for use

2. Installation

7

The keyboard is connected to the keyboard

Dos.1

The notch on the plug must coincide with the marking on the panel.

2.3 Setup

2.3.1 Connecting the keyboard

socket provided for it on the rear panel of the instrument.

2.3.2 Connecting the Dosinos

The Dosinos are connected to the sockets ”DOS1” to ”DOS4” on the rear panel of the 711 Liquino. Press each Dosino plug into the socket until it clicks into place!

A Dosino should only be connected when the instrument is switched off! The 711 Liquino only recognizes Dosinos which are already plugged in when it is switched on.

2.3.3 Connecting a Pt100 temperature sensor

711 Liquino, Instructions for use

The Pt100 temperature sensor 6.1111.030 with 4-wire technology can be used with the 711 Liquino. It is connected to the socket marked with ”Pt100” on the rear panel of the instrument.

2.4 Memory card

8

Pipet tip

Green pilot lamp

6.1562.040

Black start button

6.1562.050 Pipetting tubing

Connection to dosing port 1 of the Dosino 700

Connection cable to 711 Liquino (remote connection)

Screw nipple

2.3.4 Installing the pipetting attachment

The pipetting attachment available as an option is suitable for automatic pipetting functions with a Dosino 700.

Pipet handle

To install the pipetting attachment proceed as follows:

• Loosen the screw nipple on the pipet handle and push it over the pipet tubing.

• Guide the pipet tubing into the handle and fix the tubing with the screw nipple.

• Mount the pipet tubing on dosing port 1 of the Dosino dosing unit.

• Insert in the 25-pin connection cable plug into the remote socket of the

Liquino. The second connection cable plug is used to connect another peripheral unit to the Liquino.

• As soon as the pipet handle is connected the green pilot lamp lights up to indicate that it is ready for work.

• The angle between the tubing guide and the handle can be adjusted for strain-free work.

Important: the pipet tubing must always be clean and kink-free!

Pipetting accessories:

Pipet handle 6.1562.040

with spiral pipet tubing, 3 mL 6.1562.050

Pipet tubing, 10 mL 6.1562.100 Pipet tubing, 3 mL 6.1829.020 Pipet tubing, 0.7 mL 6.1562.010 Pipet tips for pipet tubing 0.7 mL, 10 pieces 6.1562.030 Pipet tip holder 6.2052.010

2.4 Memory card

The memory card (e.g. 6.2245.010) must be inserted in the slot on the front panel of the 711 Liquino so that the front of the memory card (with the type name) faces to the right. A little pressure is necessary to push the memory card completely into the slot. Never remove the memory card from the instrument when it is being accessed by the instrument.

711 Liquino, Instructions for use

9

RS 232

Remote

Dosimats

pH Meter / Conductometer

Titrino family

726 Titroprocessor

730 Sample changer

665 ..

691 692 712 713

702

751

Seiko

Citizen

Epson

HP

IBM

other devices e. g. thermostat

730

711 Liquino

726

700 Dosinos

Pt100

Printer

Balance

pumps

heating bath

etc.

AC

DC

731 Relay box

other devices

Dos.1-4

772 Pump unit

683 Pump

711 Liquino

pumps

heating bath

etc.

...

776

Personal computer

2. Installation

2.5 Connections

Metrohm automated systems with the 711 Liquino

711 Liquino, Instructions for use

2.5 Connections

10

Input 0

21

START

Input 1

9

STOP

Input 2

22

HOLD / CONTINUE

Input 3

10

External ready

Input 4

23

Sample Changer ready

Input 5

11

not used

Input 6

24

PIP continue

Input 7

12

not used

Output 0

5

Ready

Output 1

18

Upper limit

Output 2

4

Lower limit

Output 3

17

EOD (End of Determination)

Output 4

3

Activate 1

Output 5

16

Activate 2

Output 6

1

External start

Output 7

2

Start Sample Changer

2.5.1 Remote connections

The remote control of instruments within a Metrohm automated system can (apart from data communication via RS232 interfaces) be carried out in a simple manner with the help of parallel-switched signal leads, the remote lines (or I/O lines). Signals can be set statically or transmitted as a signal pulse (usually approx. 200 ms duration); see SCAN and CONTROL commands, (page 91ff). The signal level is +5 volt (TTL-level) in each case.

The functions which can be used for remote control or monitoring tasks each occupy a particular remote lead. The remote socket of a Metrohm instrument has input leads (Input0…7, for the control of certain functions, e.g. START or STOP) and output leads (Output0…8, to display instrument conditions, e.g. 'ready' or 'End of Determination').

The remote connection is normally a 25-pin socket. Different connection cables are available for different types of instrument. The suitable remote cable is listed in the ‘Instructions for use’ of the corresponding instrument. Special connection cables can also be made according to the customers’ particular requirements.

Remote lead occupancy for 711 Liquino:

Remote lead Pin Function

Output leads 8…13 cannot be used. In the SEQ mode remote leads Input3…7 and Output4…7 can be freely used with the commands SCAN and CONTROL (see page 91ff).

711 Liquino, Instructions for use

2. Installation

11

Note:

B

A

Titrino

C

D

230

cable 6.2141.090

Connection cables

Only Metrohm cables should be used to connect the 711 Liquino to other instruments as these are the only ones with which interference-free data transmission can be guaranteed.

Remote cables for the 711 Liquino always have a name on the end of the cable to indicate the instrument with which the particular plug is intended to be used and which connection it should be plugged in to. Example:

Titrino B

692 / 712 / 71 3

Liquino — Titrino

Cable 6.2141.090 is used in the SMPL mode. Details can be found on page 106ff. Control commands can also be used in an SEQ method, for example:

>SEQ sequence st ep 4 ( CONTROL command) pat t er n * 1* * ----

starts Titrino (start pulse)

>SEQ sequence st ep 5 ( Pause command) pause 00: 00: 01

>SEQ sequence st ep 6 ( CONTROL command) pat t ern *0**----

wait 1 s

reset remote interface

(end pulse)

>SEQ sequence st ep 7 ( SCAN command) pattern ****1---

wait for ready message from Titrino

711 Liquino, Instructions for use

2.5 Connections

12

711

B

A

Titrino

C

D

230

683 Pump Unit

I 0

683 Pump Unit

I 0

730

cable 6.2141.100

Liquino — Titrino — 683 Pump — 730 Sample Changer

Cable 6.2141.100 is used for the SMPL mode if aspiration and rinsing the titration vessel are to be carried out as quickly as possible (with 2 x Pump

683). The sample changer connection can be left open if no sample chang-

er is required. The Titrino, the pumps and the sample changer can also be addressed with the control commands of a SEQ method, for example:

Start Titrino

>SEQ sequence st ep 4 ( CONTROL command) pat t er n * 1* * ---- starts Titrino (starts pulse)

>SEQ sequence st ep 5 ( Pause command) pause 00: 00: 01

>SEQ sequence st ep 6 ( CONTROL command) pat t er n * 0* * ----

wait 1 s

starts Titrino (ends pulse)

>SEQ sequence st ep 7 ( SCAN command) pattern ****1---

wait for ready message from Titrino

Run pump 1 for 10 s

>SEQ sequence st ep 8 ( CONTROL command) pattern ***1---- switches on 1st 683 pump

>SEQ sequence st ep 9 ( Pause command) pause 00: 00: 10

wait 10 s

>SEQ sequence st ep 10 ( CONTROL command) pattern ***0----

switches off 1st pump 683 again

Run pump 2 for 1 min 5 s

>SEQ sequence st ep 11 ( CONTROL command) pat t er n * * 1* ---- switches on 2nd pump 683

>SEQ sequence st ep 12 ( Pause command) pause 00: 01: 05

wait 1 min 5 s

>SEQ sequence st ep 13 ( CONTROL command) pat t er n * * 0* ----

switches off 2nd pump 683 again

711 Liquino, Instructions for use

2. Installation

13

711

B

A

Titr

ino

C

D

7

30

cable 6.9921.165

Command to

730 Sample Changer

SCN:Rm: ready1 ←

CTL:Rm: START device1→

Switch sample changer to next sample

>SEQ sequence st ep 14 ( CONTROL command) pat t er n 1* * * ---- switches sample changer 1 sample further

*)

(start pulse)

>SEQ sequence st ep 15 ( Pause command) pause 00: 00: 01

>SEQ sequence st ep 16 ( CONTROL command) pat t er n 0* * * ----

wait 1 s

resets remote interface

(end pulse)

>SEQ sequence st ep 17 ( SCAN command) pattern ***1*---

wait for ready message from sample changer

711 Liquino – 730 Sample Changer – Titrino

730 Sample Changer with Titrino and 711 Liquino for automated pipetting of different samples on the sample changer into a special beaker on the sample rack.

The 711 Liquino can be used in any automated system for pipetting tasks (PIP mode). In this case the 730 Sample Changer controls the working process. The 711 Liquino is used in the PIP mode. The determination of the samples is carried out by the Titrino which, like the Liquino, is started from the sample changer. This arrangement of instruments requires a special remote cable (6.9921.165). Other special cables for similar instrument combinations are available on request.

*)

For this function the sample changer must be appropriately programmed with Scan and Control com-

mands!

711 Liquino, Instructions for use

2.5 Connections

14

>st ar t sequence

3 Lift: 1: shift mm

1 Lift: 1: shift mm

711

731

772

cable

6.2125.100

Dosinos

heating bath

mains cable

Example of a sample changer method:

1 CTL: Rm: INIT

>sampl e sequence 1 CTL: Rm: START devi ce1 2 SCN: Rm: r eady1

4 CTL: Rm: *********1**** 5 Wai t 1 s 6 CTL: Rm: *********0**** 7 Mov e: 1: sampl e 8 Li f t : 1: wor k mm 9 CTL: Rm: *********1**** 10 Wai t 1 s 11 CTL: Rm: *********0**** 12 SCN: Rm: r eady1 13 Mov e: 1: spec. 1 14 Li f t : 1: wor k mm 15 CTL: Rm: *********1**** 16 Wai t 1 s 17 CTL: Rm: *********0**** 18 SCN: Rm: end1 19 St i r : 1: ON s 20 CTL: Rm: START devi ce2 2 1 SCN: Rm: e nd2 22 St i r : 1: OFF s 23 Pump: 1. 1: 12 s 24 Pump: 1. * : 10 s 25 Pump: 1. 1: 12 s 28 NOP

>f i nal sequence

2 NOP

← Initialize remote interface

← Start Liquino (PIP mode) ← Wait for pipetting step ← Lift out of sample vessel ← Switch pipetting further (corresponds to

<ENTER>)

— separating bubble is aspirated —

← Reset remote interface ← Position sample beaker ← Immerse pipet tubing in sample ← Switch pipetting further (corresponds to

<ENTER>)

← Reset remote interface ← Wait for next pipetting step ← Move to titrating beaker ← Pipet tubing in titrating beaker ← Switch pipetting further (corresponds to

<ENTER>)

← Reset remote interface ← Wait for end of PIP mode ← Stirrer on ← Start Titrino ← Wait for end of determination ← Switch off stirrer ← Aspirate titration beaker ← Rinse titration beaker ← Aspirate titration beaker

— sample is aspirated —

— sample is ejected —

711 Liquino – 731 Relay Box – 772 Pump Unit – Heating Bath

Liquino with 772 Pump Unit as delivery or aspiration pump and a heating bath.

With the aid of a Metrohm 731 Relay Box the output leads of the 711 Liquino can be monitored and, according to their line conditions, two low-voltage d.c. voltage outputs and two mains voltage outputs can be switched.

In this way the heating bath can be switched automatically via the temperature monitoring function. If the measured temperature falls below a certain value the bath is heated up.

A connected pump (e.g. the Metrohm 772 Pump Unit) can be selectively switched on or off during the method procedure.

711 Liquino, Instructions for use

2. Installation

15

731 Relay Box settings:

Connect 772 Pump Unit to DC1 (or DC2) Output voltage: 18 or 24 volt Remote address selection disk DC1: 7 (=Output 7)

Connect heating bath to AC1 (or AC2, mains voltage) Remote address selection disk AC1: 2 (=Output 2)

711 Liquino settings

Temperature monitoring

XDOS mode (contained in SEQ mode):

Par amet er s >XDOS moni t or i ng t emperat ur e: on low limit xx°C upper limit ... action: ... al ar m pi ns: under

Control commands for the pump

SEQ mode

Switch on pump:

command: CONTROL i nt er f ace: Remot e

pat t er n 1* * * ---- (Output 7)

(switch off with

0***----)

711 Liquino, Instructions for use

2.5 Connections

16

cable 6.2134.040 (9-pin/9-pin) or 6.2134.050 (9

printer cables: see page 17f

711

2.5.2 Serial connections

A wide range of possible connections can be made at the RS232 interface. As well as all Metrohm instruments which are equipped with the Metrohm remote control language, a printer (requirement: serial interface or parallel/serial converter) or a personal computer (PC) can also be connected. Any instrument from another manufacturer which is equipped with a serial RS232 interface can also be connected.

-pin/25-pin)

A requirement for correct data transmission is that the transmission parameters are correctly set; these must coincide with the interface settings of the connected instrument (see following page).

Control commands (examples):

>SEQ sequence st ep 4 (Control command) st r i ng &M; $G

starts Metrohm instrument

>SEQ sequence st ep 6 (Control command) st r i ng &M; $S

stops Metrohm instrument

Input data query (example):

>SEQ sequence st ep 5 (Scan command) st r i ng * R"

wait for ready message from Metrohm instrument

The following section provides information about the settings and cables necessary to connect a printer.

711 Liquino, Instructions for use

2. Installation

17

The Liquino must be switched off before a printer is connected to the RS232 interface!

Printer

Cable

RS232 settings

Settings on printer

IBM Proprinter

6.2125.050 +

6.2125.010

baud rate: 9600 data bit: 8 stop bit: 1 Parity: none handshake: Hardware send to: IBM

see printer manual

Seiko DPU-411

6.2125.020

+

6.2125.010

baud rate: 9600 data bit: 8 stop bit: 1 parity: none handshake: Hardware send to: Seiko

DIP switch settings:

DIP01 DIP02

on

off

1 2 3 4 5 6 7 8 1 2 3 4 5 6

Depending on the set dialog language, the adjustable 7-bit ASCII character set of the printer will be set automatically to the national character set.

2.5.3 Connecting a printer

Printers with the following printer drivers can be connected:

IBM IBM Proprinter and printers with IBM emulation Epson Epson printers and printers with Epson emulation Seiko Seiko printer DPU-411 or DPU-414 Citizen Citizen printer IDP560 RS HP HP printers and printers with HP PCL3 emulation

If you wish to connect a different printer then ensure that this can emulate one of the printer modes supported by the 711 Liquino. Most printers with a serial interface are connected with cable 6.2134.050. Printers with a parallel interface require a serial/parallel converter (e.g.

2.145.0300) and cable 6.2125.020 + adapter cable 6.2125.010.

The interface parameters are entered in the configuration menu under

‘>RS232 settings’. The printer type must also be entered in the configura- tion menu under ‘>Peripheral units’ and ‘send to:’

If you use an A4 printer and the graphics do not cover the whole width of the page then you can proceed as follows: When the instrument is switched on keep the <CONFIG> key pressed down. In this way you access the setup menu. Press the <> key and <ENTER>. You can now alter the relative width and height of the graphics. In each case press <ENTER> after the entry.

The following table provides information about the connection of several selected printers.

711 Liquino, Instructions for use

2.5 Connections

18

Printer

Cable

RS232 settings

Settings on printer

Seiko DPU-414

6.2125.130

baud rate: 9600 data bit: 8 stop bit: 1 parity: none handshake: Hardware send to: Seiko

Recommended DIP switch settings:

Dip SW-1 Dip SW-2 Dip SW-3 1 OFF ON ON 2 ON OFF ON 3 ON ON ON 4 OFF ON ON 5 ON ON OFF 6 OFF ON ON 7 ON OFF ON 8 ON OFF ON

Depending on the set dialog language, the adjustable 7-bit ASCII character set of the printer will be set automatically to the national character set.

Citizen IDP562-RS

6.2125.050

baud rate: 9600 data bit: 8 stop bit: 1 parity: none handshake: Hardware send to: Citizen

DIP switch settings:

1 2 3 4 5 6 7 8 9

10

ON

SSW1

The adjustable 7-bit ASCII character set of the printer can only be set to the national character set by switching DIP switches 4 and 5 in the printer:

4 5 Character set

OFF OFF USA ON ON United Kingdom ON OFF France OFF ON Germany

No special Spanish character set is available (it is best to select French).

Epson with 6-pin round plug

6.2125.040

+

6.2125.010

baud rate: 9600 data bit: 8 stop bit: 1 parity: none handshake: Hardware send to: Epson

DIP switch settings:

SW1 SW2

on

off

1 2 3 4 5 6 7 8 1 2 3 4 5 6 7 8

Epson with additional serial interface #8148

6.2134.050

baud rate: 9600 data bit: 8 stop bit: 1 parity: none handshake: Hardware send to: Epson

DIP switch settings at interface:

SW1 SW2

on

off

1 2 3 4 5 6 7 81 2 3 4 5 6

Epson LX-300

6.2134.050

baud rate: 9600 data bit: 8 stop bit: 1 parity: none handshake: Hardware send to: Epson

see printer manual

HP Deskjet with serial interface

6.2134.050

baud rate: 9600 data bit: 8 stop bit: 1 parity: none handshake: Hardware send to: HP

DIP switch settings:

A B

on

off

1 2 3 4 5 6 7 8 1 2 3 4 5 6 7 8

HP Laserjet with serial interface

6.2134.050

baud rate: 9600 data bit: 8 stop bit: 1 parity: none handshake: Hardware send to: HP

see printer manual *

HP Deskjet/ Laserjet with parallel interface

6.2125.020 +6.2125.01 0 + serial/ parallel converter

2.145.0300

baud rate: 9600 data bit: 8 stop bit: 1 parity: none handshake: Hardware send to: HP

see printer manual *

* The printer must be set to the PC-8 character set. PCL3 command:

esc(10U

711 Liquino, Instructions for use

2. Installation

19

Balance

Cable

Sartorius MP8, MC1

6.2134.060

Mettler AB, AG (LC-RS25)

supplied with balance

Mettler AM, PM

from Mettler: ME 33995: green wire to Pin 2, brown wire to Pin 3, white wire to Pin 7, yellow wire to Pin 20 of the 25-pin plug + 6.2125.010 25-pin/9-pin adapter

Mettler interface 016

cable supplied with interface 016: red wire to Pin 3, white wire to Pin 7 of the 25-pin plug + 6.2125.010 25-pin/9-pin adapter

Mettler interface 011 or 012

6.2125.020 + 6.2125.010

Mettler AT

from Mettler: ME 33995: green wire to Pin 2, brown wire to Pin 3, white wire to Pin 7, yellow wire to Pin 20 of the 25-pin plug + 6.2125.010 25-pin/9-pin adapter

AND models ER-60, 120, 180, 182 models FR-200, 300 models FX-200, 300, 320 with RS232 interface (OP-03)

6.2125.020 + 6.2125.010

Precisa, balances with RS232C interface

6.2125.080 + 6.2125.010

711

6.2125.010

printer cable

balance cable

6.2125.030

2.5.4 Connecting a balance

The following balances can be connected to the RS232 output of the 711 Liquino:

The balance type must be preselected on the 711 Liquino with the <CONFIG> key under ‘>Peripheral units’. The weight will be transmitted as a number with up to 6 places, together with sign and decimal point. Units and control characters sent by the balance will not be transmitted.

For the simultaneous connection of printer and balance the adapter cable

6.2125.010 + with junction plug 6.2125.030 are required. If the balance only works with 7 bit and the printer only works with 8 bit then the balance parity must be set to "space" while the 711 Liquino and printer run with 8 bit, "no parity".

711 Liquino, Instructions for use

3.1 The Liquino concept

20

3 Introduction

3.1 The Liquino concept

The 711 Liquino is designed so that, together with one or more 700 Dosinos, it can automate a wide range of tasks in the laboratory. Everything which falls under the general heading of 'liquid handling', i.e. the transport of liquids in any form, belongs to its range of applications. Its functions can be divided up into three steps.

• Simple manual dosing and dispensing with up to four dosing devices.

• Automated procedures for frequently reoccurring and defined tasks. The

preset modes in the instrument are used for this. When they are appropriately set they can be stored as methods in the Liquino itself or on a memory card and can be reloaded at any time.

• Complex process sequences, which can be made up from several indi- vidual methods or modes with additional auxiliary commands as required. In this way a large number of instruments can be controlled for use in demanding analytical or synthesis units.

The practical 700 Dosinos are used as dosing instruments; they can be conveniently operated with the functions and commands of the 711 Liquino. Special functions (PREP, EMPTY) are available for preparatory work (i.e. bubble-free filling and rinsing of the tubing) and emptying dosing units when a reagent needs to be changed. In order to carry out these procedures in as comfortable and reagent-saving manner as possible you can define different types of dosing unit. As the length and diameter of the tubing used can be defined the 711 Liquino is able to calculate and then use the optimal volumes for the above-mentioned functions.

With the help of the special GLP mode the 711 Liquino can be used to validate all your dosing units, i.e. to determine their accuracy. In this way GLPconform work can be ensured and also documented. The dosing procedures in the GLP mode have been optimized and realized for the 700 Dosino in such a way that meaningful characteristic values can be determined; these allow detailed information about the accuracy of the dosing cylinder to be obtained. You can adapt the necessary limits for the assessment of the reliability of the dosing accuracy yourself to suit your requirements. The limits recommended by Metrohm are set as standard. We recommend that you use these limits.

711 Liquino, Instructions for use

3 Introduction

21

CONFIG

A

The dialog language, date and time can be set in the configuration menu.

J

ENTER

YES

• and then <> and <ENTER>.

DOS NR

SELECT

P

•

• With <ENTER> the entry ‘dialog: english’ can be accepted.

CLEAR

Q

• The number keys are used to enter the current date in the format year-

lete the entry. (The date is “year 2000 safe“!)

•

• Enter the current time and confirm it with <ENTER>.

QUIT

NO

•

3.2 Tutorial

This tutorial will introduce you step by step to the operation of the Metrohm 711 Liquino. It is arranged so that you can work through it from the beginning to the end and in this way become familiar with the most important functions of the instrument. You will be guided through each section step by step so that you will be able to carry out the simplest settings. You can also carry out further fine adjustments. The necessary information for this can be found in section 4.

3.2.1 Basic configuration

The most important basic settings are carried out as follows:

• Press <CONFIG>

Di s pl ay : conf i gur at i on >per i pher al uni t s

Di s pl ay : >auxi l i ar i es di al og: engl i sh

The colon in this menu entry indicates that parameters can be selected from a list here. Press the <SELECT> key several times in order to view the different selection possibilities and become familiar with this operating mode.

Di s pl ay : >auxi l i ar i es di al og: deut sch

Di s pl ay : >auxi l i ar i es dat e: 90- 01- 01

month-date. If a mistake is made then <CLEAR> can be used to de-

The entry is accepted with <ENTER>.

Di s pl ay : >auxi l i ar i es t i me: 01: 00: 00

Di s pl ay : >auxi l i ar i es device l abel ********

Press <QUIT> 2x in order to exit the configuration menu.

711 Liquino, Instructions for use

3.2 Tutorial

22

Except for the "Sampling dosing unit" in the SMPL mode the standard port occupancy for all modes is as follows:

Port 1: dosing unit output Port 2 (bottle): refilling opening

CONFIG

A

• Press <CONFIG> and then 3x <>.

ENTER

YES

•

DOS NR

SELECT

P

• One of the ten configurable dosing units can be selected with the

Di s pl ay : >dosi ng uni t s 1

3.2.2 Defining dosing units

In order for the complete tubing system of a Dosino to be fully filled with the reagent solution without any air bubbles the 711 Liquino must know the dimensions of the connected tubing. For this reason a dosing unit can be de-

*)

fined in the configuration menu and then selected for the method.

Di s pl ay : conf i gur at i on >dosi ng uni t s

Access the submenu ‘dosing units’ with <ENTER>.

Di s pl ay : > dosi ng uni t s dos. uni t : D1

<SELECT> key. Press <ENTER> to access the settings for the corresponding dosing unit. The index for the dosing unit is located in the top right-hand corner of the display.

Di s pl ay : >dosi ng uni t s 1 I D D1

• Enter an identification text for the dosing unit or leave the preset entry as it is. Text input is explained on page 63.

• Accept the entry with <ENTER>.

Di s pl ay : >dosi ng uni t s 1 l engt h t ube1 400 mm

• Now enter the length of tubing at Dosino port 1 (for tandem dosing including the tubing length up to the T-piece) and accept the entry with <ENTER>.

Di s pl ay : >dosi ng uni t s 1 di am. t ube1 2. 0 mm

• The inner diameter of the tubing at Dosino port 1 can be entered here and confirmed with <ENTER>.

Di s pl ay : >dosi ng uni t s 1 l engt h t ube2 250 mm

• Now enter the length of the tubing at Dosino port 2 (bottle) and accept the entry with <ENTER>.

*)

In a single method ‘standard’ can also be selected for the dosing unit used. For the modes XDOS, CONT and GLP ‘standard’ means: Port1 (dosing port): L = 40cm, D = 2mm Port2 (bottle): L = 25cm, D = 2mm.

For PIP ‘standard’ means: Port1 (pipetting tubing): L = 150cm, D = 2mm Port2 (bottle): L = 25cm, D = 2mm. For SMPL ‘standard’ means: Port1 (sample tubing): L = 40cm, D = 2mm Port2 (measuring cell): L = 16cm, D = 2mm Port3 (rinsing agent): L = 50cm, D = 2mm.

711 Liquino, Instructions for use

3 Introduction

23

di am. t ube2 2. 0 mm

QUIT

NO

• The dosing unit has now been defined. Press <QUIT> 2x to exit the

• The inner diameter of the tubing at Dosino port 2 can be entered here

and confirmed with <ENTER>.

Di s pl ay : >dosi ng uni t s 1 l engt h t ube3 0 mm

• As no tubing is connected to Dosino ports 3 and 4 the tubing lengths

must be set to 0 mm. Check this for port 3, press <ENTER> and check the value for port 4 (the diameter is not requested if the length has been set to 0 mm). Press <ENTER> again.

Di s pl ay : >dosi ng uni t s 2 I D D2

configuration menu.

711 Liquino, Instructions for use

3.2 Tutorial

24

MANUAL

MAN OFF

D

DOS NR

SELECT

P

• Now use the <DOS NR / SELECT> key to select the connected dosing

PREP

4

L

•

DOSING

7

G

START

Z

• If you now press the <START> key and hold it down then dosing will take

3.2.3 Dosing and dispensing

This is where you learn the simplest functions of the Liquino: manual dosing and dispensing.

Fit a reagent bottle with a dosing unit and a Dosino and connect the Dosino to the Liquino. Select, e.g. connection socket 'Dos. 1' or 'Dos. 2' for this. Now switch the 711 Liquino briefly off and then on again. In this way the instrument recognizes the connected Dosino. Details about setting up dosing units can be found in section 6.1.2, page

143.

Now immerse the dosing tip, which must be connected to Dosino Port 1 by tubing, in a rinsing beaker.

• Switch the Liquino to the manual operating mode. Press the <MANUAL>

key.

Di spl ay: manual r eady 0. 000 mL

device. On the 711 Liquino keyboard there are four LEDs. If you have connected the Dosino to socket ' SELECT> key once so that the LED '

Dos. 2' then press the <DOS NR /

DOS 1' lights up.

<1>

• Prepare the dosing unit by pressing the <PREP> key.

The PREP function is used to rinse the tubing and fill the dosing cylinder free from bubbles.

Di s p l ay: wast e por t : tip(1) or flask(2)?

• Now select whether the rinsing volume of the reagent solution should be

discharged via the dosing tip (connected to Dosino Port 1) or returned to the storage bottle (via filling Port 2 of the Dosino). Press <

1>.

Di spl ay: manual PREP r unni ng. . .

• The tubing is now automatically rinsed with the required volume of

reagent. Excess reagent solution is discharged into the rinsing beaker. Wait until the Liquino reports 'ready'.

Now exchange the rinsing beaker for the vessel into which you wish to carry out dosing.

• Press the <DOSING> key.

Di spl ay: man u a l DOSI NG

r eady 0. 000 mL

place when the Dosino has switched the stopcock. You will notice that the dosing speed increases slowly. If you release the <START> key and then press it down again it will again start dosing at a slow speed which is gradually increased. This behavior can be very useful when you need to dose accurately, e.g. to fill a volumetric flask up to the mark.

711 Liquino, Instructions for use

3 Introduction

25

•

J

<ENTER>

• Press the <CONFIG> key and the <> key twice.

•

START

Z

• Start dosing again by pressing the <START> key; you will see that the

FILL

5

M

•

If you do not want the dosing speed to increase or you require a quicker increase in the dosing speed then you can set this in the configuration.

A

CONFIG

2x

<ENTER>

<ENTER>

Di spl ay: conf i gur at i on >manual

• Here you will find the submenu with the settings which are effective for

manual functions.

Di spl ay: >manua l DOS1 ← dosing connection dos. uni t : def aul t

• In the first line, above right, the address of the dosing connection to

which the particular setting applies is shown. You can make different settings for each of the four dosing connections. The settings for the other dosing connections DOS2 to DOS4 are also found in this submenu. Now press the <ENTER> key three times.

Di spl ay: >manual DOS1 >>dosi ng

• If you want to alter the dosing behavior of dosing device 1 you will find

this in the second submenu '>>Dosing' after pressing the <ENTER> key as given above. If your Dosino is connected to 'Dos. 2' then press the <ENTER> key six times.

Di spl ay: >>dosi ng DOS1 r at e t ype: i ncr easi ng

• By pressing the <SELECT> key and confirming with <ENTER> you

can switch to a constant dosing speed. You should, however, leave the setting with increasing speed alone and press <ENTER>.

Di spl ay: >>dosi ng DOS1 sl ope 4

• Enter the highest value '10' for the slope of the increase of the dosing

speed. Confirm the entry with <ENTER>.

By pressing the <QUIT> key twice you will return to the display for dosing.

Di spl ay: man u a l DOSI NG r eady 3. 349 mL

dosing speed increases more rapidly and that the highest dosing speed is reached very quickly.

When the max. cylinder volume has been reached the dosing unit will be filled automatically. Filling the dosing cylinder can also be triggered manu-

711 Liquino, Instructions for use

ally by pressing the <FILL> key.

3.2 Tutorial

26

MANUAL

MAN OFF

D

• Operating the <MAN. OFF / MANUAL> key switches manual operation off

MANUAL

MAN OFF

D

• Switch the Liquino to the manual operating mode by pressing the

DOS NR

SELECT

P

•

PREP

4

L

• Prepare the dosing unit again by pressing the <PREP> key. Accustom

DISPENSE

8

H

• When you have prepared the dosing unit press the <DISPENSE> key.

CLEAR

Q

<ENTER>

START

Z

•

START

Z

• If you press the <START> key the required reagent volume will be dosed.

FILL

5

M

•

again. The Liquino is again in the basic condition.

If you want to dose a particular volume several times then select the 'Dispense' function. Proceed in a similar manner to dosing.

<MANUAL> key.

Di spl ay: manual r eady 0. 000 mL

Use the <DOS NR / SELECT> key to select the connected dosing device.

yourself to rinsing the dosing units with which you want to work by means of the 'PREP' function before you use them. This is an absolute necessity when you change the reagent. Other things which must be taken into account when a reagent is changed are mentioned below.

Di spl ay: manual DI S vol ume? 1. 0 mL

• Enter the required volume. If you do not want to dose a particular volume

or if you want to correct a faulty entry press the <CLEAR> key.

Di spl ay: manual DI S vol ume? i nf i ni t e mL

• You can enter a new value or confirm the value 'infinite'. In this case dosing

or dispensing will be carried out automatically until you press the <STOP> key.

After you have entered a value and confirmed it with <ENTER> you can start to dispense with the <START> key. You also have the possibility of first altering the dosing speed. This is set to the maximum dosing speed as standard.

Di spl ay: manual DI S r at e? max mL/ mi n

The maximum dosing speed depends on the dosing unit used and the

cylinder volume. For example, for a 10 mL cylinder it is 33.33 mL/min, for a 50 mL cylinder 166.66 mL/min. The same values apply to the filling speed of the dosing unit.

• For viscous reagent solutions you should select a lower dosing speed as

otherwise a large counterpressure could build up in the tubing during rapid dispensing.

This can be carried out several times. The 'DISPENSE' function is repetitive.

Filling the dosing cylinder can be triggered with the <FILL> key.

711 Liquino, Instructions for use

27

•

A

J

• Press the <CONFIG> key and the <> key twice.

DOS NR

SELECT

P

• Press the <SELECT> key in order to switch on automatic filling of the

QUIT

NO

• Exit the configuration menu by pressing <QUIT> twice.

START

Z

• Now dispense again by pressing the <START> key and you will see that

MANUAL

MAN OFF

D

CONFIG

<ENTER>

3 Introduction

If you want, you can configure your Liquino so that after each dispensing process the dosing cylinder is refilled automatically.

2x

Di spl ay: conf i gur at i on >manual

• Here you will find the submenu with the settings which are effective for

manual functions.

Di spl ay: >manua l DOS1 ← dosing connection dos. uni t : de f a ul t

• In the first line, above right, the address of the dosing connection to

which the particular setting applies is shown. You can make different settings for each of the four dosing connections. The settings for the other dosing connections DOS2 to DOS4 are also found in this submenu. Now press the <ENTER> key twice.

Di spl ay: >manual DOS1 auto fill: off

• The colon after the word 'fill' shows that a list of entries is available for

this menu item. In this case there are only two possibilities: 'on' and 'off'.

dosing unit. Confirm the entry with <ENTER>.

<ENTER>

2x

the dosing cylinder is automatically refilled after each dosing process.

• Pressing the <MAN. OFF / MANUAL> key switches manual operation off

again. The Liquino is again in the basic condition.

711 Liquino, Instructions for use

3.2 Tutorial

28

Warning!

EXCH

6

N

• Always press the <EXCH> key first. Only in this way will the stopcock

MANUAL

MAN OFF

D

EMPTY

3

T

EXCH

6

N

• Check whether the dosing tip is immersed in a waste beaker. Use the

3.2.4 Changing the dosing unit

A dosing device consists of a dosing unit (the green part) with a dosing cylinder (2, 5, 10, 20 or 50 mL) and the dosing drive, the Dosino 700. If you are working with different reagents then you do not need a separate dosing drive for each reagent bottle. Fit the individual reagent bottles with a dosing unit (the actual buret) and simply mount the dosing drive connected to the Liquino or dosing unit on a different reagent bottle as it is required.

Incorrect disassembly of the dosing drive can damage the dosing unit and/or the Dosino.

of the dosing unit be moved to the safe, so-called 'exchange' position. You can then loosen the dosing drive without any risk by carefully turning it counterclockwise and lifting it off. Observe the lines marked on the front of the dosing unit when doing this.

If you do not use a dosing unit for a long time or want to change the reagent we recommend that the dosing unit or the dosing cylinder and the tubing are completely emptied. This can be carried out simply and conveniently by means of the 'EMPTY' function.

<MANUAL> key to switch to manual operation. Then press <EMPTY>.

<1>, <2>

Di spl ay: empt y t o por t : tip(1) or flask(2)?

• You can now select whether the cylinder contents of the dosing unit are to

be pumped back into the reagent bottle or discharged into a waste beaker via the dosing tip. Select <1> or <2>.

• The contents of the dosing cylinder are now discharged and the tubing

emptied. Please remember that the contents of the dosing tubing at Port 1 will always be discharged via the dosing tip.

• To terminate the 'EMPTY' function the dosing cylinder is filled with air. After

pressing the <EXCH> key the dosing unit can now be carefully removed.

711 Liquino, Instructions for use

3 Introduction

29

MANUAL

MAN OFF

D

TEMP

9

I

MANUAL

MAN OFF

D

• Connect a Pt100 temperature sensor. The connection socket is on the

3.2.5 Temperature measurement

The 711 Liquino is equipped with a Pt100 temperature measuring input.

Apart from temperature-controlled dosing this means that simple manual temperature measurements can also be carried out.

rear panel of the 711 Liquino. Use the <MANUAL> key to switch to manual operation. Then press <TEMP>.

Di spl ay: manual

21. 5° C

• The measured temperature in degrees Celsius is shown immediately. The

measurement can be switched off by pressing the <MANUAL> key again.

711 Liquino, Instructions for use

3.2 Tutorial

30

*

MODE

-

X

DOS NR

SELECT

P

• The PIP mode must first be activated. This sets all method parameters

ENTER

YES

• Press <ENTER>. The instrument is now in the PIP mode.

PARAM

B

QUIT

NO

• In the submenu ‘PIP parameters’ no further entries are necessary.

J

• The next submenu is accessed with <>.

Di s pl ay : >PI P dosi ng uni t

3.2.6 PIP – precise pipetting/diluting

Example: Pipet 1mL and dilute with 9mL. Distilled water is used as the

"hydraulic“ liquid.

Preconditions / Preparation

The easiest and most accurate means of pipetting is with pipetting attachment 6.1562.040. The keyboard can be used to proceed from step to step.

Define a dosing unit which corresponds to the tubing of the Dosino used. This procedure is described on page 22. (This is not necessary if the pipet-

Method editing

ting attachment is used as this corresponds to the standard settings.)

to standard values. Press the <MODE> key and then <SELECT> until ‘PIP’ appears in the display:

Di s pl ay : mode sel ect : PI P

Di s pl ay : PIP ******** r eady 0. 000 mL

• The <PARAM> key is used to access the parameter menu, where all

the possible settings for a PIP method can be found.

Di s pl ay : par amet er s >PI P par amet er s

• The submenu ‘PIP parameters’ contains the main settings for a PIP

method. Press <ENTER> to open the submenu.

Di s pl ay : >PI P par amet er s pi pet t i ng vol . 1. 000 mL

• Enter the required pipetting volume (1 mL) and press <ENTER> to

accept the entry.

Di s pl ay : >PI P par amet er s di l ut i ng vol . 9. 000 mL

• Enter the 9 mL used as diluting volume in the example and press

<ENTER>

Press the <QUIT> key to exit the submenu.

Di s pl ay : par amet er s >PI P par amet er s

<ENTER>

Di s pl ay : par amet er s >PI P dosi ng uni t

• The submenu ‘PIP dosing unit’ is opened with <ENTER>.

711 Liquino, Instructions for use

3 Introduction

31

dr i ve uni t : DOS1

START

Z

•

ENTER

YES

• Before the Dosino is used for the first time in the new configuration the

<ENTER>

<ENTER>

<QUIT>

• The Dosino which is to be used can be selected here with <SELECT>

(DOSx refers to the connection number on the 711 Liquino). Accept with <ENTER>.

Di s pl ay : >PI P dosi ng uni t dos. uni t : def aul t

• In this menu item the 711 Liquino is informed about the tubing of the

Dosino. Press <SELECT> until the dosing unit defined in the above preparation step appears. (If the pipetting attachment is used this setting can be left as ‘standard’). Confirm with <ENTER>.

Di s pl ay : par amet er s >PI P r a t e s

• As the ‘PIP dosing unit’ submenu contains no further menu items, an

automatic return is made to the submenu selection. All necessary parameters have now been entered! The parameter menu is exited with <QUIT>.

Di s pl ay : PIP ******** r eady 0. 000 mL

If an inquiry is always to be made about the pipetting volume at the start of the method then enter the value under ‘parameters/>PIP preselections/query pip. vol.’.

Various PIP methods can also be edited and then stored in the method memory. Each of these methods can then be reloaded by pressing a few keys. The method memory is described on page 128.

Carrying out the method

When <START> is now pressed the display shows

Di s pl ay : Not pr epar ed yet ! Run PREP now?

Dosino cylinder and the complete tubing system must be filled bubblefree with reagent solution. Press <YES>.

Di s pl ay : wast e por t : t i p( 1) or f l ask ( 2) ?

<1> , <2>

• Press <1> to empty the cylinder contents through the dosing tip, or

<2> to return them to the bottle. Take care that the tip of the dosing tubing is located in a vessel. Wait until the 711 Liquino has ended the preparation (PREP). The instrument then returns to its normal state.

711 Liquino, Instructions for use

3.2 Tutorial

32

START

Z

follow the instructions shown on the display.

• From now on when <START> is pressed the method will be run im-

mediately.

*)

<ENTER>

• The pipetting process consists of several steps. For each step instruc-

tions are shown on the display. If the pipetting attachment is used then the key built into the handle can be used to switch from one step to the next. The pipetting process can also be started with it. Whenever the LED on the handle lights up the 711 Liquino is ready for the next step. Without the pipetting attachment <ENTER> must be pressed in order to carry out the next step.

• In the first step a separatory bubble is formed, which is located be-

tween the "hydraulic“ liquid (in this case water) and the sample. Just

*)

The warning about the preparation of the tubing system appears each time the mode is changed and after the instrument has been switched off and on again. If it is certain that the Dosinos used have already been prepared then press <NO> (<QUIT> key) to acknowledge the warning. The method can now be run in the normal manner by pressing <START>.

711 Liquino, Instructions for use

3 Introduction

33

3.2.7 SMPL – fully automatic sampling

The capabilities and possible uses of an SMPL method will be demonstrated by means of a complexometric titration of Ni Liquino and Titrino 716.

Chemistry

2+

The Ni ed with Na-EDTA. The detection mechanism with the Cu-ISE electrode is based on the following equilibrium equation:

ion is buffered to pH 10, complexed with Cu-EDTA and then titrat-

2+

with the help of the 711

Procedure

Cu-EDTA Cu

2+

+ EDTA

2-

2+

The presence of the Ni

ion displaces the equilibrium to the right:

2+

+ Cu-EDTA Cu

Ni

2+

+ Ni-EDTA

2+

The concentration of the Cu depends on the stability of the Ni-EDTA complex.

ion (to which the Cu-ISE electrode reacts)

The SMPL mode of the Liquino offers a fully automated sample transfer, perfect preparation of the titration cell between the individual titrations (for multiple determinations) and complete control of the Titrino. However, a corresponding method must first be created or selected in the Titrino. The Dosino at connection 1 carries out the "sampling“ processes, for which its four ports have fixed definitions.

1. Through port 1 the Liquino draws in the required amount of sample and transfers it to the titration vessel through the cylinder and port 2.

2. Solvent is drawn in through port 3 and transferred to the titration vessel for rinsing/diluting (the amount can be freely selected) – in this case H

O

2

is used.

3. The second Dosino adds the buffer (pH 10).

4. The third Dosino adds the complexing agent Cu-EDTA.

5. 30 s is allowed to elapse (this possibility exists after each reagent addition) in order to allow the complexing ion to be completely bound and to

2+

release the Cu

ions.

6. The Titrino is started via the remote lead and the sample is titrated with Na-EDTA.

At the end of the titration the "sampling“ Dosino removes the contents of the titration vessel through port 2 and transfers them to a waste container via port 4.

711 Liquino, Instructions for use

3.2 Tutorial

34

Waste Port 4

Solvent

Port 3

Titration vessel

Port 2

Sample

Port 1

A new titration can now be carried out. The number of determinations and the number of times the cell is to be rinsed out can be entered. The Liquino offers the possibility of carrying out titrations comfortably and confidently. Even if the titration cell is only rinsed out once the variations only amount to 0.01 to 0.02%. Multiple determinations at defined time intervals are also possible (e.g. periodic sampling of a sample flow).

Preconditions / Preparation

Tubing connections of the "sampling“ Dosino

The determination of the NI2+ ion by potentiometric endpoint indication can be carried out with the help of the Cu-ISE electrode. For an elegant automation of the analysis the following items are required:

• the new 711 Liquino

• 3 Dosino 700s with dosing unit 710: 20 mL and 2x 10 mL glass cylin-

ders. (20mL cylinder for "sampling“ dosing unit).

• any Titrino available (e.g. 716)

• Liquino - Titrino connection cable 6.2141.090

• one Cu-ISE electrode 6.0605.02 with electrode cable 6.2104.020

• one reference electrode 6.0726.100 (KNO

sat.) with electrode cable

3

6.2106.020

• one magnetic stirrer 728

• sampling mode equipment 6.5614.010.

711 Liquino, Instructions for use

3 Introduction

35

*

MODE

-

X

DOS NR

SELECT

P

• The SMPL mode must first be activated. This sets all method parame-

ENTER

YES

• Press <ENTER>. The instrument is now in the SMPL mode.

PARAM

B

Method editing

The dosing units which correspond to the tubing used for the Dosinos must be defined. This process is described on page 16.

ters to standard values. Press the <MODE> key and then <SELECT> until ‘SMPL’ appears in the display:

Di s pl ay : mode sel ect : SMPL

<ENTER>

Di s pl ay : SMPL ******** r eady 0. 000 mL

• The <PARAM> key is used to access the parameter menu, where all the possible settings for an SMPL method can be found.

Di s pl ay : par amet er s >SMPL par amet er s

• The submenu ‘SMPL parameters’ contains the main settings for an SMPL method. Press <ENTER> to open the submenu.

Di s pl ay : >SMPL par amet er s sampl e c ount 1

• Enter the number of samplings (or titrations), which are to be carried out after each other automatically. Accept the value with <ENTER>.

Di s pl ay : >SMPL par amet er s sampl i ng mode: manual

• If a multiple determination on the same sample is to be carried out then <SELECT> can be used to choose the entry ‘auto’. However, if a different sample is to be transferred each time then ‘manual’ should be selected. In this case the process requires the sample tubing to be immersed in the new sample each time. Press <ENTER>.

Di s pl ay : >SMPL par amet er s t i me i nt er val 00: 05: 00

• This parameter determines the time interval between successive sam- ples. For a multiple determination this value should be set to 00:00:00. In this way the next sample will be transferred at the end of the titration. Press <ENTER> to accept the value.

Di s pl ay : par amet er s >SMPL sampl i ng oper at i on

• As the ‘SMPL parameters’ submenu contains no further menu items, an automatic return is made to the submenu selection. The submenu ‘SMPL sampling operation' contains the parameters for sample transfer. Press <ENTER> to open it.

Di s pl ay : >SMPL sampl i ng oper at i on sampl e v ol ume 3 mL

• Enter the volume of the sample to be transferred to the measuring cell (in this case 3 mL). Press <ENTER> to accept the value.

Di s pl ay : >SMPL sampl i ng oper at i on

711 Liquino, Instructions for use

3.2 Tutorial

36

di l ut i on vol . 3 mL

QUIT

NO

• As the remaining parameters in this submenu can be left at their preset

J

<ENTER>

•

<ENTER>

• The dilution volume is the amount of solvent to be added to the meas-

uring cell after the sample has been transferred there (in the example 3 mL). Press <ENTER> to accept the value.

Di s pl ay : >SMPL sampl i ng oper at i on sampl e r i nse vol . 3 mL

• Before the actual sample transfer the Dosino cylinder is rinsed with the

sample. This rinsing volume should be about the same as the transfer amount (in the example 3 mL). For a multiple determination, in which the same sample is always used, this volume can also be smaller. Press <ENTER> to accept the value.

Di s pl ay : >SMPL sampl i ng oper at i on sampl e r i nse r ep. 1

• Enter how often the cylinder is to be rinsed with the sample. If samples

are being transferred which do not greatly differ from one another 1 rinse is sufficient. Press <ENTER> to accept the value.

values it can be exited with the <QUIT> key.

Di s pl ay : par amet er s >SMPL sampl i ng oper at i on

The next submenu is accessed with <>.

Di s pl ay : par amet er s >SMPL meas. c el l r i ns i ng

• Press <ENTER> to open the submenu ‘SMPL meas.cell rinsing.

<ENTER>

Di s pl ay : >SMPL meas. cel l r i nsi ng ext er nal Pump: of f

• The cell can also be rinsed with external pumps. However, the same

Dosino is to be used here. Press <ENTER> to accept the default value ‘off’.

Di s pl ay : >SMPL meas. cel l r i nsi ng r i nsi ng r epet i t i ons 1

• Enter the number of times that the measuring cell is to be rinsed. As

this process takes a considerable time this value should be kept as low as possible. In this example 1 rinse is sufficient. Press <ENTER> to accept the value.

Di s pl ay : >SMPL meas. cel l r i nsi ng aspi r . vol ume 40 mL

• The suction volume corresponds to the sample volume + dilution vol-

ume (solvent) + titrant consumption. The value must be so large that the measuring cell is completely emptied after the titration. In this case the total volume amounts to 40 mL. Press <ENTER> to accept the value.

Di s pl ay : >SMPL meas. cel l r i nsi ng aspi r . r at e max mL/ mi n

• This setting is left at ‘max’. It only requires alteration for viscous liquids.

Press <ENTER>.

711 Liquino, Instructions for use

37

before

after

3 Introduction

<ENTER>

<ENTER>

<ENTER>

<ENTER>

Di s pl ay : >SMPL meas. cel l r i nsi ng r i nsi ng vol ume 30. 0 mL

• The amount of solvent to be used to rinse the measuring cell is entered here. In this example 30 mL are sufficient. Press <ENTER> to accept the value.

Di s pl ay : >SMPL meas. c el l r i nsi ng r i ns. r at e max mL/ mi n

• The measuring cell should be rinsed as rapidly as possible, so that the rate can be left at ‘max’. Press <ENTER>.

Di s pl ay : par amet er s >SMPL dosi ng uni t s

• As the ‘SMPL meas. cell rinsing’ submenu contains no further menu items, an automatic return is made to the submenu selection. The submenu ‘SMPL dosing units' contains the parameters for the auxiliary dosing units and the tubing of the "sampling“ dosing unit. The addition of the pH 10 buffer and the Cu-EDTA are defined here. The submenu is opened with <ENTER>.

Di s pl ay : >SMPL dosi ng uni t s dos. uni t 1: def aul t

• Here the tubing of the "sampling" dosing unit defined during the prepa- rations is selected. The "sampling“ dosing unit must be connected to connection DOS1 of the Liquino. Press <SELECT> until the correct entry appears and accept it with <ENTER>.

Di s pl ay : >SMPL dosi ng uni t s >>aux. sol ut . BEFORE

• The double arrow (>>) shows that <ENTER> can be used to open a further lower submenu. The auxiliary solution which is to be added directly only an auxiliary solution to be added

the sample transfer can be defined here. In this example

the sample transfer is

needed. Press <>.

Di s pl ay : >SMPL dosi ng uni t s >>aux. sol ut . AFTER

• <ENTER> is used to open the next lower submenu ‘>>aux. solut. AFTER'. The auxiliary solution which is to be added directly sample transfer is defined here.

Di s pl ay : >>aux. sol ut . AFTER no1 dr i ve uni t : of f

• Use <SELECT> to choose the Dosino which is to contain the pH 10 buffer (e.g. DOS2) and press <ENTER>.

Di s pl ay : >>aux. sol ut . AFTER no1 dos. uni t : def aul t

• Here the tubing of the "sampling" dosing unit defined during the prepa- rations is selected for the Dosino with pH 10 buffer. Press <SELECT> until the correct entry appears and accept it with <ENTER>.

Di s pl ay : >>aux. sol ut . AFTER no1 vol ume 1. 000 mL

• Enter the volume which is to be added (in this example 1 mL). Accept

the

711 Liquino, Instructions for use

3.2 Tutorial

38

the value with <ENTER>.

ed is 1.000 mL, the waiting time 00:00:20 (20 s).

2x <QUIT>

<ENTER>

<>

<ENTER>

<ENTER>

Di s pl ay : >>aux. sol ut . AFTER no1 f eed r at e max mL/ mi n

• The rate of addition for the pH 10 buffer can be entered here. The max-

imum rate (default) is already correct. Press <ENTER>.

Di s pl ay : >>aux. sol ut . AFTER no1 f i l l r at e max mL/ mi n

• This is the rate at which the Dosino cylinder will be refilled. The default

value (max) can be accepted with <ENTER>.

Di s pl ay : >>aux. sol ut . AFTER no1 wai t t i me 00: 00: 00

• After the auxiliary solution has been added a waiting period can be

entered. However, this is not necessary after the addition of the pH 10 buffer. <ENTER> is used to accept the default value (00:00:00). In this way the definition of the first auxiliary solution addition is completed.

Di s pl ay : >>aux. sol ut . AFTER no2 dr i ve uni t : of f

• The second auxiliary solution can now be defined. The above steps are

repeated, this time for the addition of Cu-EDTA. The volume to be add-

• The definition of the auxiliary solutions has now been completed. Press

<QUIT> 2x to return to the upper level of the submenu.

Di s pl ay : par amet er s >SMPL dosi ng uni t s

• <> is used to open the next submenu.

Di s pl ay : par amet er s >SMPL cont r ol I / O

• The submenu ‘>SMPL control I/O’ defines the interaction of the Liqui-

no with other instruments (e.g. Titrino). It is opened with <ENTER>.

Di s pl ay : >SMPL cont r ol I / O sampl e c hanger ct r l : of f

• Press <ENTER> to accept the default values.

Di s pl ay : > S MPL cont r ol I / O ext . dev i ce ct r l : of f

• Use <SELECT> to choose the entry ‘on’ and confirm it with

<ENTER>.

Di s pl ay : >SMPL cont r ol I / O st ar t ext . devi ce: r emot e

• An external instrument can be addressed by both the Remote and the

RS interface. In this example it is easier to control the Titrino via the remote interface. The default value is accepted with <ENTER>.

Di s pl ay : >SMPL cont r ol I / O Ans wer bac k f r om: Remot e

• The prompt from the Titrino after the titration should also be requested

via the remote interface. Confirm the default value with <ENTER>.

711 Liquino, Instructions for use

3 Introduction

39

<ENTER>

the SMPL method.

START

Z

•

ENTER

YES

• Before the Dosino is used for the first time in the new configuration the

START

Z

Di s pl ay : par amet er s >SMPL pr esel ect i ons

• As the ‘SMPL control I/O’ submenu contains no further menu items, an

<QUIT>

Various SMPL methods can be edited and then stored in the method memory. Each of these methods can then be reloaded by pressing a few keys. The method memory is described on page 128.

Running the method

Di s pl ay : Not pr epar d yet ! Run PREP now?

automatic return is made to the submenu selection. The parameter menu is exited with <QUIT>. The instrument is now ready to carry out

When <START> is now pressed the display shows

Dosino cylinder and the complete tubing system must be filled bubblefree with the particular reagent solution. Press <YES>.

Di s pl ay : wast e por t : t i p( 1) or f l ask ( 2) ?

• Press <1> to empty the contents of the cylinder through the dosing tip or <2> to return them to the bottle. Take care that the tip of the dosing tubing is located in a vessel. Wait until the 711 Liquino has ended the preparation (PREP) of all the Dosinos which are being used. The instrument then returns to its normal state.

• From now on when <START> is pressed the method will be run im- mediately.

*)

The warning about the preparation of the tubing system appears each time the mode is changed and after the instrument has been switched off and on again. If it is certain that the Dosinos used have already been prepared then press <NO> (<QUIT> key) to acknowledge the warning. The method can now be run in the normal manner by pressing <START>.

711 Liquino, Instructions for use

3.2 Tutorial

40

Example:

*

MODE

-

X

DOS NR

SELECT

P

•

ENTER

YES

•

PARAM

B

3.2.8 CONT – the automatic volumetric flask

A typical daily task is the preparation of standard solutions. Preparing serial dilutions is often time-consuming and involves making calculations. The CONT/volume fraction mode of the 711 Liquino allows this monotonous routine work to be automated.

drinking water by ion chromatography. The sample to be determined has chloride content of about 10 ppm. The standard concentrations should be in the range 5 - 15 ppm.

Pipetting and adding the standard solution is no longer necessary as the dosing device (Dosino 700) can be screwed directly on to the bottle containing the standard solution. All that needs to be done is to inform the instrument of the concentration of the standard solution and required target volume (volumetric flask mark). After the start the instrument will request the entry of the final content. The corresponding amount of standard solution is added automatically to the volumetric flask which then only needs to be filled up to the mark. At the next start the next concentration in the serial dilution is entered.

Preconditions / Preparation

the preparation of a standard for the determination of chloride in

Method editing

Define a dosing unit which corresponds to the tubing of the Dosino used. This procedure is described on page 22.

The CONT mode must first be activated. This sets all method parameters to standard values. Press the <MODE> key and then <SELECT> until ‘CONT’ appears in the display:

Di spl ay: mode sel ect : CONT

Press <ENTER>. The instrument is now in the CONT mode.

Di s pl ay : CONT ******** r eady 0. 000 mL

• The <PARAM> key is used to access the parameter menu, where all

the possible settings for a CONT method can be found.

Di s pl ay : par amet er s >CONT par amet er s

• The submenu ‘>CONT parameters’ contains the main settings for a

CONT method. Press <ENTER> to open the submenu.

Di s pl ay : >CONT par amet er s t ype: s ubst . conc .

• The colon indicates that the <SELECT> key can be used to select a

value from a list. Press <SELECT> until ‘volume fraction’ appears.

Di s pl ay : >CONT par amet er s

t ype: v ol ume f r act i on

711 Liquino, Instructions for use

3 Introduction

41

•

Accept the entry with <ENTER>.

Di s pl ay : >CONT par amet er s meas . uni t : mol / L

• Use the <SELECT> key to choose ‘ppm’ and confirm the entry with

<ENTER>.

Di s pl ay : >CONT par amet er s t ar get vol ume 10. 0 mL

• The target volume corresponds to the volumetric flask volume up to the

mark. In this example enter ‘10’ and confirm this value with <ENTER>.

Di s pl ay : >CONT par amet er s cont ent s t d. 1. 000 ppm

• Enter the standard solution content (in this example 1000 ppm). Press

<ENTER> to accept the entry.

Di s pl ay : par amet er s >CONT dosi ng uni t

• As the ‘>CONT parameters’ submenu contains no further menu items,

the next submenu automatically becomes available. Open it with <ENTER>.

Di s pl ay : >CONT dosi ng uni t dr i ve uni t : DOS1

• The Dosino to be used can be chosen with <SELECT> (DOSx refers

to the connection number on the 711 Liquino). Press <ENTER> to accept the entry.

Di s pl ay : >CONT dosi ng uni t dos. uni t : def aul t

• In this menu item the 711 Liquino is informed about the tubing of the

Dosino. Press <SELECT> until the dosing unit defined in the above preparation step appears. Confirm with <ENTER>.

Di s pl ay : par amet er s >CONT r at es

• All the necessary parameters have now been entered. The parameter

menu is exited with the <QUIT> key.

711 Liquino, Instructions for use

3.2 Tutorial

42

START

Z

•

ENTER

YES

• Before the Dosino is used for the first time in the new configuration the

START

Z

A CONT method can be edited and stored in the method memory for each standard solution. Each of these methods can then be reloaded by pressing a few keys. The method memory is described on page 128.

Running the method

When <START> is now pressed the display shows

Di s pl ay : Not pr epar ed yet ! Run PREP now?

Dosino cylinder and the complete tubing system must be filled bubblefree with the reagent solution. Press <YES>.

Di s pl ay : wast e por t : t i p( 1) or f l ask ( 2) ?

• Press <1> to empty the contents of the cylinder through the dosing tip

or <2> to return them to the bottle. Take care that the tip of the dosing tubing is located in a vessel. Wait until the 711 Liquino has ended the preparation (PREP) of all the Dosinos which are being used. The instrument then returns to its normal state.

• From now on when <START> is pressed the method will be run im-

mediately.

• The instrument requires the target content to be entered. As soon as

*)

the entry is confirmed with <ENTER> the required volume is calculated and added.

*)

The warning about the preparation of the tubing system appears each time the mode is changed and after the instrument has been switched off and on again. If it is certain that the Dosinos used have already been prepared then press <NO> (<QUIT> key) to acknowledge the warning. The method can now be run in the normal manner by pressing <START>.

711 Liquino, Instructions for use

3 Introduction

43

*

MODE

-

X

DOS NR

SELECT

P

•

ENTER

YES

•

PARAM

B

• Enter the volume which is to be added (1000 mL in this example) and

QUIT

NO

•

Di s pl ay : par amet er s

3.2.9 XDOS – the electronic dropping funnel

120mL of solution are to be added in 5 hours. This can be carried out easily and reliably with a tandem addition using 2 Dosinos. In this way interruptionfree addition is guaranteed.

Preconditions / Preparation

The accessories for tandem addition (see ”ordering information” in the ”711 Liquino” leaflet) are required for the tubing. However, it is also possible to lead a separate tubing from each Dosino to the test apparatus.

A dosing unit which corresponds to the tubing used for the Dosino must be defined. This process is described on page 22.

Method editing

The XDOS mode must first be activated. This sets all method parameters to standard values. Press the <MODE> key and then <SELECT> until ‘XDOS’ appears in the display:

Di s pl ay : mode sel ect : XDOS

Press <ENTER>. The instrument is now in the XDOS mode.

Di s pl ay : XDOS ******** r eady 0. 000 mL

• The <PARAM> key is used to access the parameter menu, where all

the possible settings for an XDOS method can be found.

Di s pl ay : par amet er s >XDOS par amet er s

• The submenu ‘XDOS parameters’ contains the main settings for an

XDOS method. Press <ENTER> to open the submenu.

Di s pl ay : >XDOS par amet er s XDOS t ype: vol ume&r at e

• The colon indicates that the <SELECT> key can be used to select a

value from a list. Press <SELECT> until ‘volume&time’ appears. Accept the entry with <ENTER>.

Di s pl ay : >XDOS par amet er s vol ume 1. 000 mL

press <ENTER>.

Di s pl ay : >XDOS par amet er s dosi ng t i me 00: 01: 00

• Enter the length of time for the addition in ‘hours:minutes:seconds’

format (if a mistake is made press the <CLEAR> key and repeat the entry). Accept the value with <ENTER>.

Di s pl ay : >XDOS par amet er s

t emp. measur i ng: of f

Exit with the <QUIT> key.

No further entries are necessary in the ‘XDOS parameters’ submenu.

711 Liquino, Instructions for use

3.2 Tutorial

44

J

>XDOS par amet er s

• No further entries are required for the task to be carried out. Exit the

parameter menu with <QUIT>.

• <> is used to open the next submenu.

Di s pl ay : par amet er s >XDOS dosi ng uni t s

• Press <ENTER> to access the submenu ‘XDOS dosing units'.

Di s pl ay : >XDOS dosi ng uni t s set up: s i ngl e

• Use the <SELECT> key to choose the entry ‘tandem’ and confirm it

with <ENTER>.

Di s pl ay : >XDOS dosi ng uni t no. 1 dr i ve uni t : DOS1

• The first of the two Dosinos can now be entered with <SELECT>

(DOSx refers to the connection number on the 711 Liquino). Accept with <ENTER>.

Di s pl ay : >XDOS dosi ng uni t no. 1 dos. uni t : def aul t

• In this menu item the 711 Liquino is informed about the tubing of the

Dosino. Press <SELECT> until the dosing unit defined in the above preparation step appears. Confirm with <ENTER>.

• Skip the next menu item with <ENTER>.

Di s pl ay : >XDOS dosi ng uni t no. 2 dosi ng dr i ve: DOS2

• Now repeat the entry for the second Dosino. Select the same dosing

Di s pl ay : par amet er s >XDOS moni t or i ng

unit again. After the entry has been made for the second Dosino the submenu ‘>XDOS dosing unit’ is terminated and the next submenu is displayed.

711 Liquino, Instructions for use

3 Introduction

45

START

Z

• When <START> is now pressed the display shows

ENTER

YES

• Before the Dosino is used for the first time in the new configuration the

START

Z

Various XDOS methods can be edited and stored in the method memory. Each of these methods can then be reloaded by pressing a few keys. The method memory is described on page 128.

Running the method

Di s pl ay : Not pr epar ed yet ! Run PREP now?

Dosino cylinder and the complete tubing system must be filled bubblefree with the reagent solution. Press <YES>.

Di s pl ay : Put t i p i n vess el ! Run PREP?

• Take care that the tip of the dosing tubing is located in a vessel and

then press <YES>. Wait until the 711 Liquino has ended the preparation (PREP). The instrument then returns to its normal state.

• From now on when <START> is pressed the method will be run im-

mediately.

*)

The warning about the preparation of the tubing system appears each time the mode is changed and after the instrument has been switched off and on again. If it is certain that the Dosinos used have already been prepared then press <NO> (<QUIT> key) to acknowledge the warning. The method can now be run in the normal manner by pressing <START>.

711 Liquino, Instructions for use

3.2 Tutorial

46

Example:

*

MODE

-

X

DOS NR

SELECT

P

• The XDOS mode must first be activated. This sets all method parame-

ENTER

YES

•

3.2.10 XDOS – temperature-controlled addition

hydrochloric acid is to be added to 0.1 mol freshly distilled aniline. During this process the temperature of the mixture should, if possible, not exceed 10°C. The 711 Liquino will carry out the reagent addition and control the temperature.

Preconditions / Preparation

To carry out the above task the following items are required:

• the new 711 Liquino

• a Dosino 700 with a 50 mL dosing unit 710

• a printer with cable if the process is to be documented (see page 12)

• a four-neck flask with precision glass stirrer shaft

• a cooling device (if an appropriate cooling bath is used this can even be

A dosing unit which corresponds to the tubing used for the Dosino must be defined. This process is described on page 22.

Screw the Dosino 700 on to the bottle containing hydrochloric acid, place the 0.1 mol aniline in the four-neck flask and carry out the method described below under intensive stirring. The flask must be cooled continuously. If the temperature limit of 10 °C is exceeded the Liquino immediately stops the HCl addition. As soon as the temperature sinks below 10 °C again the

Liquino continues with the addition

Method editing

during the preparation for a nitration 0.3 mol semi-concentrated

switched on and off by the Liquino via the remote interface).

*)

.

ters to standard values. Press the <MODE> key and then <SELECT> until ‘XDOS’ appears in the display:

Di s pl ay : mode sel ect : XDOS

Press <ENTER>. The instrument is now in the XDOS mode.

Di s pl ay : XDOS ******** r eady 0. 000 mL

*)

An upper and lower temperature limit can be defined as well as the action to be taken when these limits are

exceeded. Possible actions are:

• none (limit violations are only mentioned in the report)

• stop

• switch instrument to HOLD condition (restart with <CONTINUE>)

• stop, wait until the temperature is again within the limits and then continue automatically.

711 Liquino, Instructions for use

3 Introduction

47

PARAM

B

• Enter the volume which is to be added (90 mL in this example) and

•

Press <ENTER> to confirm the entry.

QUIT

NO

J

<ENTER>

• The <PARAM> key is used to access the parameter menu, where all

the possible settings for an XDOS method can be found.

Di s pl ay : par amet er s >XDOS par amet er s

• The submenu ‘XDOS parameters’ contains the main settings for an

XDOS method. Press <ENTER> to open the submenu.

Di s pl ay: >XDOS par amet er s XDOS Type: vol umen&r at e

• Press <ENTER> to accept the default value.

Di s pl ay : >XDOS par amet er s vol ume 1. 000 mL

<ENTER>

<ENTER>

press <ENTER>.

Di s pl ay : >XDOS par amet er s f eed r at e max mL/ mi n

• Enter the feed rate (in this example 50 mL/min). Accept the value with

<ENTER>.

Di s pl ay : >XDOS par amet er s t emp. meas ur i ng: of f

The colon indicates that the <SELECT> key can be used to select a value from a list. Press <SELECT> until ‘on’ appears and confirm the entry with <ENTER>.

Di s pl ay : >XDOS par amet er s meas . i nt er val 00: 01: 00

• The time interval at which a measurement is to be added to the list of

measuring points can be determined here. This is used for the graphics, the list of temperature measurements and the combined measurement list report. The interval at which the temperature is measured for controlling the temperature is not dependent on this value but is carried out every second.

• No further entries are necessary in the ‘XDOS parameters’ submenu.

Exit with the <QUIT> key.

Di s pl ay : par amet er s >XDOS par amet er s

• <> is used to open the next submenu.

<ENTER>

Di s pl ay : Par amet er >XDOS dosi ng uni t s

• Press <ENTER> to access the submenu ‘XDOS dosing units’.

Di s pl ay : >XDOS dosi ng uni t s set up: s i ngl e

<ENTER>

711 Liquino, Instructions for use

• As only 1 Dosino is needed the default value can be confirmed with

<ENTER>.

Di s pl ay : >XDOS dosi ng uni t s dr i ve uni t : DOS1

• The Dosino to be used can be entered with <SELECT> (DOSx refers

to the connection number on the 711 Liquino). Accept with <ENTER>.

Di s pl ay : >XDOS dosi ng uni t s

3.2 Tutorial

48

<ENTER>

dos. uni t : st andar d

• In this menu item the 711 Liquino is informed about the tubing of the

Dosino. Press <SELECT> until the dosing unit defined in the above

<ENTER>

<ENTER>

preparation step appears. Confirm with <ENTER>.

• Skip the next menu item with <ENTER>.

Di s pl ay : par amet er s >XDOS moni t or i ng

• As the submenu ‘>XDOS dosing units' does not contain any further

menu items, an automatic return is made to the submenu selection. Press <ENTER> to open the submenu ‘>XDOS monitoring'.

Di s pl ay : >XDOS moni t or i ng t emper at ur e: of f

• Use the <SELECT> key to select the entry ‘on’. This activates the

temperature monitoring.

Di spl ay: >XDOS moni t or i ng

low limit - 70 ° C

• The lower temperature limit is of no interest in this application. Accept

the default value with <ENTER>.

Di s pl ay : >XDOS moni t or i ng upper l i mi t 200 ° C

• Set the upper temperature limit to 10 °C. Confirm the entry with

<ENTER>.

Di s pl ay : >XDOS moni t or i ng act i on: none

<ENTER>

<QUIT>

2x <>

• The action to be taken if the temperature exceeds the set limits is de-

termined here. Use <SELECT> to choose the entry ‘wait’. This stops any addition when the temperature is outside the limits. When the temperature again lies within the limits the addition will be continued. Accept the setting with <ENTER>.

• No further entries are necessary in the ‘XDOS monitoring’ submenu.

Exit with the <QUIT> key.

Di s pl ay : par amet er s XDOS moni t or i ng

• Press <> 2x to switch to the submenu ‘XDOS reports’.*)

Di s pl ay : par amet er s >XDOS r epor t s

• Press <ENTER> to open the submenu.

Di s pl ay : >XDOS r epor t s t emp. aut o scal e: on

*)

If no printer or PC is connected the parameter menu can be exited with <QUIT> and the method rejoined

at "Running the method“.

711 Liquino, Instructions for use

3 Introduction

49

•

All the necessary parameters have now been entered!

<ENTER>

2x <QUIT>

In this menu item <SELECT> can be used to choose whether a temperature curve should be scaled automatically or manually. Accept the default value ‘on’ with <ENTER>.

Di s pl ay : >XDOS r epor t s no. 1 r epor t : of f

• The <SELECT> key can be used to select from the following reports:

• ‘off’: no report

• ‘results’: summary of the results

• ‘parameters’: parameter settings

• ‘curve’: graph of the measurements and additions

• ‘V-list’: list of volume measuring points

• ‘T-list’: list of temperature measuring points

• ‘comb. list': combined volume/temperature measuring point list

• ‘ff’: page feed (may be useful between 2 reports)

Select the reports to be printed out and press the <ENTER> key after each selection. Up to 8 entries can be made. Press <QUIT> 2x to exit the parameter menu.

Various XDOS methods can be edited and stored in the method memory. Each of these methods can then be reloaded by pressing a few keys. The method memory is described on page 128.

711 Liquino, Instructions for use

3.2 Tutorial

50

START

Z

•

ENTER

YES

• Before the Dosino is used for the first time in the new configuration the

START

Z

Running the method

When <START> is now pressed the display shows

Di s pl ay : Not pr epar ed yet ! Run PREP now?

Dosino cylinder and the complete tubing system must be filled bubblefree with the reagent solution. Press <YES>.

Di s pl ay : Put t i p i n vess el ! Run PREP?

• Take care that the tip of the dosing tubing is located in a vessel and

then press <YES>. Wait until the 711 Liquino has ended the preparation (PREP). The instrument then returns to its normal state

• From now on when <START> is pressed the method will be run im-

mediately.

*)

The warning about the preparation of the tubing system appears each time the mode is changed and after the instrument has been switched off and on again. If it is certain that the Dosinos used have already been prepared then press <NO> (<QUIT> key) to acknowledge the warning. The method can now be run in the normal manner by pressing <START>.

711 Liquino, Instructions for use

3 Introduction

51

Example:

3.2.11 SEQ – complex procedures under control

thesis procedure might read as follows:

" 0.3 mol of a semi-concentrated hydrochloric acid is added to 0.1 mol freshly distilled aniline. The temperature should remain below approx. 10°C. After cooling the mixture to 0°C a 0.1 mol solution of NaNO that temperature does not exceed 5°C. When this addition is complete 8% β-naphthol solution (2 molar) is added. The temperature should not exceed approx. 10°C.“

This procedure can be broken down into the following steps:

1. Temperature-controlled addition of semi-concentrated hydrochloric acid

2. Pause for 5 minutes for cooling down to 0 °C.

3. Temperature-controlled diazotization (temperature below 5 °C).

4. Pause for 1 minute.

5. Temperature-controlled azo coupling (temperature below approx. 10 °C)

The individual additions with temperature control can be carried out by an XDOS method. However, the SEQ mode is available to automate the complete procedure. It allows individual XDOS and also other methods to be combined with each another. Pauses between steps and the control of other instruments are also possible.

Preconditions / Preparation

the preparation of phenolazonaphthol. A short version of the syn-

to aniline (temperature below approx. 10 °C).

with β-naphthol.

is added so

2

Method editing

The following instruments and accessories are required:

• the 711 Liquino

• 3 Dosino 700s, each with a 50 mL dosing unit 710

• a printer with cable if the process is to be documented (see page 12)

• a four-neck flask

• a cooling device (if an appropriate cooling bath is used this can even be

switched on and off by the Liquino via the remote interface).

Dosing units which correspond to the tubings of the Dosinos used must be defined. This process is described on page 22.

For the three temperature-controlled additions three different XDOS methods must be defined, each of these stored under "USER METHOD“ and then selected at the appropriate step in the SEQ method. Storing a method which has been edited is described on page 64.

The way in which the first XDOS method (addition) is created can be found in the section "XDOS – temperature-controlled addition“ on page 46.

711 Liquino, Instructions for use

3.2 Tutorial

52

For the other two XDOS methods (diazotization and azo coupling) the parameter lists are printed out below. Use these lists together with the practical experience already gained to enter the parameters. Lines marked with

( adapt ) must be adapted to the existing conditions.

XDOS method for diazotization

711 Li qui no 711. 0011 dat e 1998- 07- 08 t i me 18: 16 mode: XDOS user met hod: NaNO2add par amet er s >XDOS par amet er XDOS t ype: vol ume&r at e vol ume 80. 0 mL f eed r at e 30. 0 mL/ mi n t emp. measur i ng on r ec. i nt er val 00: 01: 00 f i l l r at e max mL/ mi n aut o f i l l on >XDOS dosi ng uni t s set up: si ngl e dosi ng dr i ve: DOS2 dos. uni t : Na NO2

( adapt ) ( adapt )

por t use: def aul t >XDOS moni t or i ng t emper at ur e: on low limit - 70 ° C upper l i mi t 4. 0 ° C act i on: wai t al ar m pi ns: none vol ume: of f >XDOS pr esel ect i ons r eq. i dent : of f >>XDOS pr ompt s i d1 I d1 i d2 I d2 i d3 I d3 st ar t del ay 00: 00: 00 >XDOS r epor t s t emp. aut o scal e: on r epor t 1: r esul t

(with printer, if not: off)

r epor t 2: cur ve (with printer, if not: off) r epor t 3: of f r epor t 4: of f r epor t 5: of f r epor t 6: of f r epor t 7: of f r epor t 8: of f ============

711 Liquino, Instructions for use

3 Introduction

53

XDOS method for azo coupling

711 Li qui no 711. 0011 dat e 1998- 07- 08 t i me 18: 42 mode: XDOS user met hod: AZZOc oup par amet er s >XDOS par amet er XDOS t ype: vol ume&r at e vol ume 400. 0 mL f eed r at e 30. 0 mL/ mi n t emp. measur i ng on r ec. i nt er val 00: 01: 00 f i l l r at e max mL/ mi n aut o f i l l on >XDOS dosi ng uni t s set up: si ngl e dosi ng dr i ve: DOS3 ( adapt ) dos. uni t : AZO1 ( adapt ) por t use: def aul t >XDOS moni t or i ng t emper at ur e: on low limit - 70 ° C upper l i mi t 10. 0 ° C act i on: wai t al ar m pi ns: none vol ume: of f >XDOS pr esel ect i ons r eq. i dent : of f >>XDOS pr ompt s i d1 I d1 i d2 I d2 i d3 I d3 st ar t del ay 00: 00: 00 >XDOS r epor t s t emp. aut o scal e: on r epor t 1: r esul t

(with printer, if not: off)

r epor t 2: cur ve (with printer, if not: off) r epor t 3: of f r epor t 4: of f r epor t 5: of f r epor t 6: of f r epor t 7: off r epor t 8: of f ============

711 Liquino, Instructions for use

3.2 Tutorial

54

*

MODE

-

X

DOS NR

SELECT

P

• The SEQ mode must first be activated. This sets all method parameters

ENTER

YES

• Press <ENTER>. The instrument is now in the SEQ mode.

PARAM

B

Di s pl ay : >SEQ sequence st ep 4

<ENTER>

<ENTER>

<ENTER>

SEQ method editing

As the sub-methods have now been defined and stored, the SEQ method can now be assembled.

to standard values. Press the <MODE> key and then <SELECT> until ‘SEQ’ appears in the display:

Di s pl ay : mode sel ect : SEQ

Di s pl ay : SEQ ******** r eady 0. 000 mL

• The <PARAM> key is used to access the parameter menu, where all

the possible settings for a SEQ method can be found.

Di s pl ay : par amet er s >SEQ s equence

• In the submenu ‘SEQ sequence’ previously defined and stored XDOS

methods can be assembled to form a sequence and the corresponding pauses inserted. Press <ENTER> to open the submenu.

Di s pl ay : >SEQ sequence st ep 1 command: NO OPERATI ON

• "1. Temperature-controlled acidification of aniline with semi-

concentrated hydrochloric acid (temperature below approx. 10 °C)“.

Use the <SELECT> key to choose the command ‘METHOD’ and confirm with <ENTER>.

Di s pl ay : >SEQ sequence st ep 1 met hod:

Press the <SELECT> key until the name of the method which has been stored for the acidification appears. Press <ENTER> to accept the selection.

Di s pl ay : >SEQ sequence st ep 2 command: NO OPERATI ON

<ENTER>

• "2. Pause for 5 minutes for cooling down to 0 °C.“

The <SELECT> key can now be used to select the command ‘PAUSE’ and confirm it with <ENTER>.

Di s pl ay : >SEQ sequence st ep 2 pause 00: 00: 00

Enter a pause of ’00:05:00’. (If a mistake is made press the <CLEAR> key to delete the value and repeat the entry.)

Di s pl ay : >SEQ sequence st ep 3 command: NO OPERATI ON

<ENTER>

• "3. Temperature-controlled diazotization (temperature below 5 °C).“

Select the command ‘METHOD’ as in step 1 and then the XDOS method which has been stored for diazotization. Confirm each with <ENTER>.

711 Liquino, Instructions for use

3 Introduction

55

command: NO OPERATI ON

state.

<>

<>

<HOME>

<END>

<INSERT> shifts the current and all subsequent steps downwards by one

<ENTER>

• "4. Pause for 1 minute.“

Proceed as in step 2: select the command ‘Pause’ and enter ’00:01:00’. Press <ENTER> to accept the entry.

Di s pl ay : >SEQ sequence st ep 5 command: NO OPERATI ON

<ENTER>

2x <QUIT>

• "5. Temperature-controlled azo coupling (temperature below approx. 10

°C).“

Select the command ‘METHOD’ and then the XDOS method which has been created and stored for the azo coupling. Confirm each step with <ENTER>.

Di s pl ay : >SEQ sequence st ep 6 command: NO OPERATI ON

• All the necessary entries have now been made. Press the <QUIT> key

2x to exit the parameter menu. The instrument is now in its normal

When working on a sequence it is possible to switch rapidly between steps which have already been entered or to insert or delete a step with the aid of the following keys (provided that the program is in the command selection of a step, e.g.

and

command: PAUSE):

change to the next and previous command respectively.

go to the first and last command respectively.

position and inserts a ‘NO OPERATION’ command.

wards by one position.

deletes the current step and shifts all subsequent steps up-

711 Liquino, Instructions for use

3.2 Tutorial

56

START

Z

• When <START> is now pressed the display shows

ENTER

YES

•

START

Z

Running the method

Di s pl ay : Not pr epar ed yet ! Run PREP now?

Before the Dosino is used for the first time in the new configuration the Dosino cylinder and the complete tubing system must be filled bubblefree with the particular reagent solution. Press <YES>.

Di s pl ay : wast e por t : t i p( 1) or f l ask ( 2) ?

• Press <1> to empty the contents of the cylinder through the dosing tip

or <2> to return them to the bottle. Take care that the tips of the dosing tubing is located in a vessel. Wait until the 711 Liquino has ended the preparation (PREP) of all the Dosinos which are being used. The instrument then returns to its normal state.

• From now on when <START> is pressed the method will be run im-

mediately.

*)

The warning about the preparation of the tubing system appears each time the mode is changed and after the instrument has been switched off and on again. If it is certain that the Dosinos used have already been prepared then press <NO> (<QUIT> key) to acknowledge the warning. The method can now be run in the normal manner by pressing <START>.

711 Liquino, Instructions for use

3 Introduction

57

:

3.2.12 GLP – automatic validation

For the automatic validation of a Dosino or the dosing unit a balance be connected to the 711 Liquino via the RS interface (see also page 19). In the GLP mode the Liquino automatically adds liquid to a tared vessel on the analytical balance, calculates the volume of the liquid added and compares this with the theoretical volume. The validation protocol is printed out on the connected printer in agreement with GLP practice. The liquid used in this example is distilled water, which has advantages when used for this test.

Preconditions / Preparation

The connection of the printer and balance is described on pages 17 and 19.

A dosing unit which corresponds to the tubing of the Dosino used must be defined. This process is described on page 22.

The following instruments and accessories must be available:

*)

must

• dosing tubing on Port 1 of the Dosino with buret tip 6.1543.060 (without

diffusion-reducing valve)

• bottle filled with degassed water onto which the Dosino is screwed

• analytical balance, resolution 0.1 mg

• narrow-neck Erlenmeyer flask

• calibrated thermometer.

Make the following preparations:

• Measure the temperature of the water to be added. Set up the test appa-

ratus so that it is not exposed to direct sunlight or draughts. The series of measurements must be carried out without any interruption.

• Mount the buret tip firmly on a support rod. It must not be moved during

the test. If possible lead the buret tip into the balance chamber directly from above (cover the top of the balance chamber). Place the Erlenmeyer flask on the balance.

It is important that during the addition the stream of liquid breaks off

cleanly each time. This means that special precautions must be taken for some cylinder volumes:

attach a yellow Eppendorf pipet tip to the buret tip. Insert a piece of

2mL

absorbent cotton in the Erlenmeyer flask and fasten the buret tip so that it just does not touch the wad of cotton.

5, 10, 20 mL: attach a yellow Eppendorf pipet tip to the buret tip. 50 mL: attach a blue Eppendorf pipet tip to the buret tip.

*)

It is also possible to work without any direct connection between the balance and Liquino. The correspond-

ing weight must then be entered via the keyboard.

711 Liquino, Instructions for use

3.2 Tutorial

58

*

MODE

-

X

DOS NR

SELECT

P

• The GLP mode must first be activated. This sets all method parameters

ENTER

YES

• Press <ENTER>. The instrument is now in the GLP mode.

PARAM

B

Creating the GLP method

to standard values. Press the <MODE> key and then <SELECT> until ‘GLP’ appears in the display:

Di s pl ay : mode sel ect : GLP

<ENTER>

<ENTER>

<ENTER>

Di s pl ay : GLP ******** r eady 0. 000 mL

• The <PARAM> key is used to access the parameter menu, where all

the possible settings for a GLP method can be found.

Di s pl ay : par amet er s >GLP par amet er s

• The submenu ‘GLP parameters’ contains the main settings for a GLP

method. Press <ENTER> to open the submenu.

Di s pl ay : >GLP par amet er s dr i ve uni t : DOS1

• The Dosino which is to be used can be chosen here with <SELECT>

(DOSx refers to the connection number on the 711 Liquino). Press <ENTER> to accept the entry.

Di s pl ay : >GLP par amet er s dos. uni t : def aul t

• In this menu item the 711 Liquino is informed about the tubing of the

Dosino. Press <SELECT> until the dosing unit defined in the above preparation step appears.

Di s pl ay : >GLP par amet er s t emper at ur e 20. 00 ° C

• Enter the temperature of the water to be added here. This value should

be as accurate as possible as it is used to calculate the density of the water. Press <ENTER> to accept the value.

Di s pl ay : par amet er s >GLP opt i ons

• As the ‘>GLP parameters’ submenu contains no further menu items,

an automatic return is made to the submenu selection. Press <ENTER> to open the submenu ‘GLP options’.

Di spl ay: >GLP opt i ons

l i qui d: wat er

• Press <ENTER> to confirm that "water" is the liquid to be added.

Di s pl ay : >GLP opt i ons wei ght f r om: bal ance

• Use <ENTER> to confirm that the balance is connected to the RS

interface and that the weight will be transmitted by the balance.

*)

If the balance cannot be or is not to be connected to the RS interface then the <SELECT> key should be used to choose the entry ‘keyboard’. During the procedure each weight must be read off from the balance and entered via the Liquino keyboard. (The next menu item ‘Balance-Id’ is skipped in this case!)

711 Liquino, Instructions for use

3 Introduction

59

<ENTER>

Di s pl ay : >GLP opt i ons bal ance- Id

• Enter an unambiguous identification for the balance used (e.g. serial

number). The input of text is explained on 63.

Di s pl ay : par amet er s >GLP r epor t s

• As the ‘GLP options’ submenu contains no further menu items, an

automatic return is made to the submenu selection. Press <ENTER> to open the submenu ‘GLP reports’. The reports which are to be printed out automatically at the end of the GLP test are defined here.

Di s pl ay : >GLP r epor t s no. 1 r epor t : of f

• The <SELECT> key can be used to select from the following reports:

• ‘off’: no report

• ‘result’: summary of the results

• ‘parameter’: parameter settings

• ‘curve’: graph of the measurement

• ‘detail’: results in detail with list of measuring points

• ‘ff’: page feed (may be useful between 2 reports)

<ENTER>

Select the reports to be printed out and press the <ENTER> key after each selection. Up to 5 entries can be made.

Press <QUIT> 2x to exit the parameter menu.

All the necessary parameters have now been entered!

2x <QUIT>

Various GLP methods can be edited and stored in the method memory. Each of these memories can then be reloaded by pressing a few keys. The method memory is described on page 128.

711 Liquino, Instructions for use

3.2 Tutorial

60

START

Z

• When <START> is now pressed the display shows

ENTER

YES

•

START

Z

• Press <START> again. The test procedure begins. Just follow the

Running the GLP method

<1> or <2>

Di s pl ay : Not pr epar ed yet ! Run PREP no?

Before a GLP test it is absolutely necessary that the Dosino cylinder and the complete tubing system must be filled bubble-free with reagent solution. Press <YES>.

Di s pl ay : wast e por t : t i p( 1) or f l ask ( 2) ?

• Press <1> to empty the contents of the cylinder through the dosing tip

or <2> to return them to the bottle. Take care that the tips of the dosing tubing is located in a vessel. Wait until the 711 Liquino has ended the preparation (PREP) of all the Dosinos which are being used. The instrument then returns to its normal state.

instructions show on the display!

711 Liquino, Instructions for use

4. Detailed description

61

71 1 Li quino Cont rol l er

DOS 1

DOS 2

DOS 4

DOS NR

QUIT

ENTER

DOS ING DISPENSE

TEMP

PREP

EXCH

CUR DATA

EMPTY

MEM CARD

.

PRINT

*

CONTINUE

6

.214

2.0

20

STOP

START

Me

t

ro

hm

DOS 3

MODE

FILL

ALPHA

HOLD

0

3

21

6

54

9

87

CLEAR

END

HOME

MANUAL

INSERT SELECT

DELETE

CONFIG PARA M

USER

METHO D

-

YES

NO

MAN OFF

A

B C

D

E F

G

H

I

J

K

L

M N

O

P

Q

R

S

T

U

V

Y

W

X

Z

Menu keys

Editing and

Manual Action keys

Dosing device

4 Detailed description

4.1 The keyboard

LEDs

navigating

functions

The dosing device LEDs indicate the active dosing device. In manual operation the dosing device can be selected with the <SELECT / DOS NR> key.

Liquino 711, Instructions for use

4.1 The keyboard

62

CONFIG

A

USER

METHO D

C

CONTINUE

HOLD

Y

STOP

START

Z

E

J

HOME

F

END

K

ALPHA

INSERT

O

DELETE

U

DOS NR

SELECT

P

4.1.1 Menu keys

Opens the configuration menu. For details see page 69.

B

Opens the parameter menu. For details see page 74ff.

PARAM

Opens the method storage menu. For details see page 128. See also < MEM CARD> key.

4.1.2 Action keys

Interrupts an automatic procedure or continues it again.

Stops an automatic procedure.

Starts a method or a manual function.

4.1.3 Editing and navigating keys

Cursor keys for rapid navigation in menus and submenus. Does not exit from submenu automatically.

Selects the first or last entry in a menu or submenu.

Selects character set for text input by repeatedly pressing the <ALPHA> key. With the following possibilities:

• number input (directly via the numeric block of the keyboard)

• capital letters (directly via the keyboard), display: ALPHA

• lower case letters (directly via the keyboard), display: alpha

• special characters 1 and 2 (input via the numeric block)

Inserts an empty command line or deletes a command line in the SEQ mode.

Selects an entry from a selection list during editing.

In manual mode: selects the active dosing device (DOS 1…4).

Liquino 711, Instructions for use

4. Detailed description

63

QUIT

NO

CLEAR

Q

ENTER

YES

MANUAL

MAN OFF

D

DOSING

7

G

DISPENSE

8

H

TEMP

9

I

PREP

4

L

FILL

5

M

EXCH

6

N

CUR DATA

1

R

EMPTY

3

T

MEM CARD

0

V

Exits a submenu or confirms an error message.

Completely deletes an entry during editing or deletes the last character in the text input mode.

Confirms an entry during editing. Opens a submenu during navigating.

Switches on (or switches off) manual operation.

4.1.4 Manual functions and other keys

Manual dosing. This function is only available in the manual mode, see <MANUAL> key.

Manual dispensing of a particular volume. This function is only available in the manual mode, see <MANUAL> key.

Manual temperature measurement with a Pt100 temperature sensor. This function is only available in the manual mode, see <MANUAL> key.

Manual preparation of a dosing unit.

Manual filling of a dosing unit.

Moves 4-way stopcock of dosing unit to exchange position. Must be carried out each time before a dosing drive is disassembled.

Input of sample-specific data (ID1…3). Only possible in automatic mode.

Completely empties a dosing unit.

Accesses memory card.

• Loads methods, stores them or deletes them

• Changes directory, makes or deletes directory

• Saves all methods or reloads

• Formats card or changes battery

Liquino 711, Instructions for use

4.1 The keyboard

64

.

PRINT

W

*

MODE

-

X

Prints out various reports.

Selects an automatic run mode:

• XDOS - controlled dosing

• PIP - pipetting

• CONT - preparation of solutions

• SMPL - automated sampling

• SEQ - sequential procedures

• GLP - validation mode for dosing units

Selection is made either with the <SELECT> key or by repeatedly pressing the <MODE> key.

Liquino 711, Instructions for use

4. Detailed description

65

ENTER

YES

J

HOME

F

END

K

ENTER

YES

CLEAR

Q

QUIT

NO

DOS NR

SELECT

P

ALPHA

4.2 Editing

The instrument dialog system of the Liquino 711 is chiefly organized as a menu system. For example, the <CONFIG> key forms the access to the configuration menu of the basic settings and the <PARAM> key provides access to the parameters of a run mode or a method. The menus are further split up into submenus.

4.2.1 Navigating in menus

• Use the <ENTER> key to view and process the individual lines in a menu.

Di spl ay: conf i gur at i on >pe r i pher al uni t s

• Submenu titles are marked with a '>' character. Use the <ENTER> key

to access a submenu.

You can also navigate in menus with the cursor keys <> and <>.

•

No data will be altered and no submenus opened.

In order to reach the first or last menu item in a menu or submenu as

•

quickly as possible use the <HOME> or <END> keys.

•

4.2.2 Data input

• Numerical inputs can be entered easily with the number block of the key-

• An incorrect entry can be corrected with the <CLEAR> key. This always

Di spl ay: >XDOS par amet er f eed r at e max mL/ mi n

• A data input can be aborted with <QUIT>. This restores the previous

• Most menu items allow parameters to be selected from a selection list. By

Di spl ay: >auxi l i ari es di al og: engl i s h

The <QUIT> key is available to access the next higher level from a submenu or to reach the basic condition from a main menu.

board. Confirm each input with the <ENTER> key.

sets the so-called CLEAR value; a special value e.g. 'max' or 'infinite'.

value.

repeatedly pressing the <SELECT> key the individual entries in the list can be selected. These entries must also be confirmed with <ENTER>.

• Menu items which offer a selection list are indicated by a colon; see

above.

• Some menu items require a text input. Switch the alphanumeric text editor

on. Press the <ALPHA> keys. Details about text input are given below.

Liquino 711, Instructions for use

4.2 Editing

66

Key

Sign

Key

Sign

Key

Sign

<0>

?

<3>

"

<7>

'

<1>

empty

<4>

$

<8> =

space

<5>

%

<9>

^

<2>

!

<6> & = esc-sign

Key

Sign

Key

Sign

Key

Sign

<0>

@

<4>

+

<8>

/

<1>

(

<5>

,

<9>

#

<2>

)

<6> ; <3>

*

<7> _

4.2.3 Text input

The text editor can be used wherever a text input is required. Numbers can be entered directly.

The <ALPHA> key can be used to switch between four sets of characters.

• Capital letters (ALPHA character set)

• Lower case letters (alpha character set)

• Special character set 1

• Special character set 2

The individual characters can then be entered directly via the keyboard. Observe the red printing on the keys. Special characters are entered with the number block of the keyboard. The set of special characters is always shown in the first line of the display. Each special character occupies a numeric key:

1st special character set:

Di spl ay: 0?1 2! 3"4$5%6&7' 8=9esc

Number key occupancy:

2nd special character set:

Di spl ay: 0@1( 2) 3* 4+5, 6; 7_8/ 9#

Number key occupancy:

Liquino 711, Instructions for use

4. Detailed description

67

>st or e met hod

First press the <CLEAR> key to delete the current contents.

ALPHA

The keyboard letters are now active. ‘ALPHA’ is in capi-

capital letters. Enter 'HC'.

al pha

Press the <ALPHA> key again to allow lower case let-

(‘alpha’ is now in lower case letters). Type in 'l'.

al pha 1 2! 3“4$5%6&7’ 8=

The next time <ALPHA> is pressed the 1st special

Press e.g. key <1> to insert an empty space.

al pha 1( 2) 3* 4+5, 6- 7. 8/

Press <ALPHA> a second time; the second special

Press e.g. key <1> to insert an open parenthesis.

>st or e met hod met hod: HCl ( 

Pressing the <ALPHA> key again exits the text editor.

>st or e met hod met hod: HCl ( 1m)

CLEAR

Q

retain their standard functions.

Example:

method: ********

ALPHA

Open the text editor with the <ALPHA> key.

met hod: 

met hod: HC

met hod: HCl

met hod: HCl 

tal letters, i.e. all letters entered will appear as

ters to be entered.

character set will appear.

If, for example, you want to add. ‘1m)’ then you must

press the following keys: <1>, 2x <ALPHA>, <M>, 2x <ALPHA>, <2> and the <ENTER> key to accept the text entry.

In order to delete a character press the <ALPHA> key until the display 'ALPHA' or 'alpha' vanishes from the 1st line of the display and no special character set is shown either. The <CLEAR> key now has its original function and deletes the last character entered (backspace function). Numbers can also be entered here.

The <QUIT> , <ENTER> and <STOP> keys always

Liquino 711, Instructions for use

4.3 Configuration

68

10 ml

Port 1

From below

Front view

Port 3

Port 2

Port 4

0 = venting

↑ Port 2

4.3 Configuration

In order for the different modes and commands of the Liquino 711 to function properly it is essential that it is configured carefully. In particular, the definition of the different types of dosing unit and the serial RS 232 interface require special care.

4.3.1 Defining the dosing units

Depending on your requirements you can fit your dosing units with tubing of different lengths and thicknesses. This results in different tubing volumes. These tubing volumes must be taken into account in the various automatic run modes and the manual operation commands <PREP> and <EMPTY> for the Liquino. This is why you should define your own dosing unit type for any dosing unit which is not equipped with the standard tubing. This is not necessary if you only work with the standard tubing.

The standard tubing:

Port 1: length 400 mm, diameter 2.0 mm Port 2: length 250 mm, diameter 2.0 mm Port 3: not fitted Port 4: not fitted

(dosing port)

(filling port)

Liquino 711, Instructions for use

4. Detailed description

69

A

CONFIG

lish

4.3.2 The configuration menu

Please note: menu entries with a colon offer a selection list. Press the <SELECT> key to make your selection.

>peripheral units >auxiliaries >manual >dosing units

>RS232 settings >report header >GLP error limits

Di spl ay I ni t i al val ue

>per i pher al uni t s

The specification of the externally connected instruments is extremely important for the correct functioning of the Liquino in an automated system. Instead of a printer a computer or other instrument (e.g. a Metrohm titrator) can be connected to the serial RS232 interface, in order to store Liquino reports or realize complex remote control functions. The is done by selecting the setting '

send t o: I BM'.

If your type of printer is not listed select 'IBM' or 'Epson'; for laser printers select 'HP'. If your balance is not listed select 'Precisa'.

send t o: I BM

bal ance: Sa r t or i us

>auxi l i ar i es

The configuration settings are retained even when the instrument is switched off.

di al og: eng

dat e 1998- 09- 11

t i me 08: 10: 15

devi c e l abel XXXXXXXX

pr ogr am 711. 0011

di spl ay cont r ast 3

beeper : on

PREP r emi nder : on

>manual

These settings are only effective in manual operation, i.e. for dosing and dispensing.

In order for the PREP and EMPTY functions to work properly the type of dosing device must be given for each dosing device which is connected. When the type of dosing unit is specified the corresponding tubing dimensions as defined under 'Configuration>Dosing units' will be used for the internal calculation of the rinsing volume.

By navigating with the <ENTER> key the settings for all 4 dosing device connections can be made one after the other.

dos. uni t : def aul t

fill rate ma x mL / mi n

aut o f i l l : of f

>>dosi ng

r at e t ype: i n cr easi ng

sl ope 4

(only for increasing dosing rate)

Input range Explanation

Type of instrument connected (RS232 interface)

IBM, Epson, Seiko, Citizen, HP printer type

Sartorius, Mettler, Mettler AT, AND, Precisa

balance manufacturer

Basic Liquino settings

english, german dialog language

JJJJ-MM-TT system date

SS:mm:ss system time

8 ASCII characters instrument identification

not editable software version number

0…7 LCD display contrast

on; off beeper for warnings and error messages

on; off automatic request to prepare the dosing units.

Settings for manual operation

selection list, see '>dosi ng

uni t s

'

0.001…166.666 mL/min; max the maximum filling rate depends on the volume of the

on; off automatic filling after dosing.

type of dosing unit connected.

dosing cylinder.

Submenu for dosing behavior

increasing; constant increases dosing rate for precise manual dosing .

1…10 slope of increase in dosing rate.

Liquino 711, Instructions for use

4.3 Configuration

70

length of tubing at Dosino Port 1 (dosing port)

length of tubing at Dosino Port 2 (filling port, dipping tubing in the bottle)

length of tubing at Dosino Port 3 (free port)

length of tubing at Dosino Port 4 (waste port in bottle)

>dosi ng uni t s

If dosing units with different lengths and diameters of tubing are used which do not correspond to the standard dimensions then special types of dosing units can be defined (max. 10). If such a dosing unit is used then its name must be entered under 'Configuration>Manual operation' or in the method with which it is to be used.

dos. uni t : D1

ID D1

l engt h t ube1 400 mm

di am. t ube1 2. 0 mm

l engt h t ube2 250 mm

Configuration of dosing units

selection list, see 'ID' below selects dosing unit.

12 ASCII characters as wished name of type of dosing unit

0…9999 mm

0.1…9.0 mm diameter of tubing at Port 1

0…9999 mm

di am. t ube2 2. 0 mm

l engt h t ube3 0 mm

l engt h t ube4 0 mm

>RS232 s et t i ngs

It is absolutely essential that the settings at the RS232 interface are in agreement with the corresponding data transmission parameters of the instrument connected.

baud r at e: 9600

dat a bi t s: 8

st op bi t s: 1

par i t y: none

handshake: Ha r dwa r e

RS cont r ol : on

>r epor t header

H1

H2

H3

>GLP er r or l i mi t s

>>err. limits 2mL- cyl .

er r or max. v ol . +/ - 6 µL

sl ope +/ - 0. 003

i nt er cept +/ - 6 µL

>>err. limits 5mL- cyl .

er r or max. v ol . +/ - 15 µL

sl ope +/ - 0. 003

i nt er cept +/ - 15 µL

>>er r . l i mi t s 10mL- cyl .

er r or max. v ol . +/ - 30 µL

sl ope +/ - 0. 003

i nt er cept +/ - 20 µL

0.1…9.0 mm diameter of tubing at Port 2

0…9999 mm

Serial RS232 interface settings

300; 600; 1200; 2400; 4800; 9600; 19200; 38400; 57600

7; 8 number of data bits

1; 2 number of stop bits

even; odd; none type of parity check

Hardware; SWChar; SWline; none

on; off blocks data reception

data transmission rate

type of handshake

Definition of the user-defined report header

21 ASCII characters as wished contents of first header line

21 ASCII characters as wished contents of second header line

21 ASCII characters as wished contents of third header line

Configuration of the error limits in the GLP test mode

Submenu for 2 mL dosing units

1…999 µL maximum volume error

0.001…0.1 maximum variation in slope

1…99 µL maximum y-axis intercept

Submenu for 5 mL dosing units

1…999 µL maximum volume error

0.001…0.1 maximum variation in slope

1…99 µL maximum y-axis intercept

Submenu for 10 mL dosing units

1…999 µL maximum volume error

0.001…0.1 maximum variation in slope

1…99 µL maximum y-axis intercept

Liquino 711, Instructions for use

4. Detailed description

71

CONFIG

A

set up

open submenu with <ENTER>

set up >gr aphi cs pr i nt out

use <> or <> to move up or down by 1 menu item

set up >show/ hi de modes

use <HOME> or <END> to jump to first or last menu item use <QUIT> to return to the basic condition

set up

Locks keyboard or particular keys

Navigate with <ENTER>

>ke yboar d opt i ons

Switches off keyboard

on

off

= the Liquino cam only be operated via external software.

>>er r . l i mi t s 20mL- cyl .

er r or max. v ol . +/ - 60 µL

sl ope +/ - 0. 003

i nt er cept +/ - 30 µL

>>er r . l i mi t s 50mL- cyl .

er r or max. v ol . +/ - 150 µL

sl ope +/ - 0. 003

i nt er cept +/ - 50 µL

Submenu for 20 mL dosing units

1…999 µL maximum volume error

0.001…0.1 maximum variation in slope

1…99 µL maximum y-axis intercept

Submenu for 50 mL dosing units

1…999 µL maximum volume error

0.001…0.1 maximum variation in slope

1…99 µL maximum y-axis intercept

4.3.3 Keyboard and graphics options

Further configuration possibilities are available:

• Locking the keyboard when the Liquino 711 is operated exclusively by

remote control.

• Locking individual dialog ranges

• Settings for graphics printout

• Hiding individual instrument modes

These settings can be made in a special setup menu which is only accessible when the Liquino is switched on with the <CONFIG> key pressed down.

Switch the Liquino off, press down the <CONFIG> key and keep this

pressed down while you switch the instrument on again.

Main menu:

>ke yboar d opt i ons

Submenus:

>ke yboar d opt i ons

l ock keyboar d: of f

If the keyboard is locked the setup menu is still available to switch off the keyboard lock.

Liquino 711, Instructions for use

4.3 Configuration

72

>ke yboar d opt i ons

Locks <CONFIG> key

on

= configuration menu is not available

>keyboard opt i ons

Locks <PARAM> key

on

= Parameters cannot be altered

>ke yboar d opt i ons

Submenu for locking the memory functions. Press <ENTER>.

>>user met hods

Locks method loading

on

= no methods can be loaded from the internal

>>user met hods

Locks method storage

on

= no methods can be stored in the internal meth-

>>user met hods

Locks method delete

on

= no methods can be deleted in the internal

>ke yboar d opt i ons

Switches off display during operation via remote control

on

= the display remains locked until the Liquino is switched

set up

Settings for printing out curves

Navigate with <ENTER>

>gr aphi cs pr i nt out

Width of the curve printout, referred to the page format of the printer

0.3…1.00

>gr aphi cs pr i nt out

Height of the curve printout, referred to the page formatof the printer

0.3…1.00

set up

Visibility of the individual modes

Navigate with <ENTER>

l ock conf i gur at i on: of f

off

l ock paramet er s of f

off

>>user met hods

The settings in this submenu only affect the internal method memory. The memory card can still be used. Memory cards can be protected against accidental erasure by activating the write protection switch on the card itself. Please read the information given on the sheet accompanying the memory card.

l ock met hod r ecal l : of f

>gr aphi cs pr i nt out

l ock met hod st or e: of f

l ock met hod del et e: of f

l ock di spl ay: of f

method memory

off

od memory

off

method memory

off

off. However, it can be operated via the remote control, see ‘Remote Control Reference'.

off

r el at i ve wi dt h 0. 50

r el at i ve hei ght 0. 50

>show/ hi de modes

Liquino 711, Instructions for use

4. Detailed description

73

>show/ hi de modes

Hides XDOS mode

yes

= the XDOS mode cannot be selected

>show/ hi de modes

Hides PIP mode

yes

= the PIP mode cannot be selected

>show/ hi de modes

Hides CONT mode

yes

= the CONT mode cannot be selected

>show/ hi de modes

Hides SMPL mode

>show/ hi de modes

Hides SEQ mode

yes

= the SEQ mode cannot be selected

>show/ hi de modes

Hides GLP mode

yes

= the GLP mode cannot be selected

hi de XDOS : no

no

hi de PI P : no

no

hi de CONT : no

no

hi de SMPL : no

yes

= the SMPL mode cannot be selected

no

hi de SEQ : no

hi de GLP : no

no

Liquino 711, Instructions for use

4.4 XDOS mode - controlled dosing

74

Task:

Vol

[mL]

t

[HH:MM:SS]

constant

dosing rate

filling time

Vol

[mL]

t

[HH:MM:SS]

constant

dosing rate

Task:

Vol

[mL]

t

[HH:MM:SS]

filling time

Vol [mL]

t

[HH:MM:SS]

4.4 XDOS mode - controlled dosing

The XDOS mode (= Extended Dosing) of the 711 Liquino allows controlled dosing of liquids with variable parameters. In principle it is possible to select one of three different types of dosing. If continuos dosing is required a tandem dosing setup can be used, i.e. dosing is carried out with a combination of two Dosinos so that while one Dosino is being filled the other Dosino carries out the dosing and vice versa.

Depending on the type of task one of the types of dosing listed below can be used:

• Volume&Rate — you enter the volume to be dosed and the required dosing rate. Filling times

lengthen the dosing process.

Volume and dosing rate

Simple dosing

Tandem dosing

• Volume&Time — you enter the volume and the time in which this volume is to be dosed (par-

ticularly suitable for synthesis applications). The dosing rate is automatically optimized by the Liquino. The filling times of the dosing units are taken into account.

Volume and time

Simple dosing

Tandem dosing

For tasks (volume and time) which cannot be fulfilled with the maximum dosing rate the 'max.

rate' will be used.

711 Liquino, Instructions for use

4. Detailed description

75

Cylinder vol.

Max. dosing rate 2 mL

6.66 mL/min

5 mL

16.66 mL/min

10 mL

33.33 mL/min

20 mL

66.66 mL/min

50 mL

166.66 mL/min

Task:

Vol

[mL]

t

[HH:MM:SS]

constant

dosing rate

filling time

Vol

[mL]

t

[HH:MM:SS]

constant

dosing rate

2 mL

6.66 mL/min

approx. 170 mL/h

5 mL

16.66 mL/min

approx. 430 mL/h

10 mL

33.33 mL/min

approx. 890 mL/h

20 mL

66.66 mL/min

approx. 1.7 L/h

50 mL

166.66 mL/min

approx. 4.3 L/h

The following equation can be used to estimate whether the max. dosing rate will be used:

Dosi ng r at e = r equi r ed del i ver y r at e ( i n mL/ mi n) ∗ 2. 22

If the required dosing rate exceeds the max. dosing rate for the selected dosing unit (or cylinder

volume) then a larger dosing unit must be selected.

The limits of the individual dosing units:

• Time&Rate — you enter the time for which dosing is to be carried out at the preselected dos-

ing rate. Filling times are taken into account.

Time and rate

Simple dosing

Tandem dosing

Delivery rate To calculate the effective delivery rate of the Liquino the cylinder volume and the filling times of the dosing unit must be taken into account. The max. delivery rates of the various dosing units:

Cylinder volume Max. dosing rate Max. delivery rate

711 Liquino, Instructions for use

Tandem dosing Tandem dosing with two dosing devices is used for continuos dosing. While one dosing device is filling its cylinder again after having dosed in a cylinder volume, the second dosing device takes over the dosing. The Dosinos work alternately.

4.4 XDOS mode - controlled dosing

76

2 mL

5.10 mL/min

approx. 300 mL/h

5 mL

12.75 mL/min

approx. 760 mL/h

10 mL

25.50 mL/min

approx. 1.5 L/h

20 mL

51.00 mL/min

approx. 3.0 L/h

50 mL

127.5 mL/min

approx. 7.6 L/h

4

2

1

3

Standard occupancy

use ' speci al ' .

However, in order to ensure interruption-free dosing the following points must be taken into account:

• In order to keep the filling times as short as possible use the highest fill-

ing rate permitted. Take the liquid viscosity and density into account.

• The dosing rate must not exceed 85% of the filling rate value. At the max.

filling rate this corresponds to the following values:

Cylinder volume Max. dosing rate Max. delivery rate

For continuous dosing the dosing rate corresponds to the delivery rate.

Monitoring functions Further options extend the dosing modes mentioned above so that you can adapt the dosing process to meet your own individual requirements:

• Temperature control: The built-in temperature measurement input

(Pt100) allows the temperature in a reaction vessel to be monitored during the dosing process. The temperature monitoring function allows the dosing to be interrupted, delayed or terminated if set temperature limits are exceeded or undercut. In addition, external instruments can be switched via remote leads.

• Volume control: In order to prevent e.g. a vessel from overflowing it is

possible to set an absolute stop volume which, when reached, immediately and unconditionally terminates the dosing. This is particularly useful for Time&Rate dosing, where the volume is not set in advance.

Documentation

For documentation of the dosing procedure a result report, a volume/temperature curve or measuring point list can be printed out or sent to a computer. To complete the documentation three lines of identification text can be entered (see example of report on page 81).

Port occupancy of the dosing units in the XDOS mode

Port 1 Dosing port Port 2 Filling port (with dipper tube) Port 3 empty Port 4 Waste (for PREP-function)

The port allocation can be altered under

>dosi ng uni t por t

711 Liquino, Instructions for use

4. Detailed description

77

paramet er s

Open submenu with <ENTER>

paramet er s

Use <> or <> to move down or up from one menu point to the next

paramet er s >XDOS moni t or i ng

Use <HOME> or <END> to jump to first or last menu point

paramet er s >XDOS pr esel ect i ons

Return to basic condition with <QUIT>

paramet er s

Dosing parameter settings.

Navigate with <ENTER>

>XDOS par amet er

ume&r at e

Selection of task parameters

volume&rate,

= selection of volume and dosing rate

>XDOS pa r amet er

Dosing volume

0.0…99999.9,

not for time&rate

>XDOS par amet er

Dosing rate

0.001…166.66,

The dosing rate is the adjustable piston stroke speed when discharging the

count.

>XDOS par amet er

Time selected for complete dosing process. Filing times must be taken into account.

HH:MM:SS

in hours, minutes and seconds (corrections can be made

>XDOS par amet er

Temperature measurement (compulsory for temperature-controlled dosing)

on, off

>XDOS par amet er

Recording interval for temperature measurement

HH:MM:SS

in hours, minutes and seconds

Depending on the

4.4.1 XDOS mode parameters

B

PARAM

All settings in the parameter menu form a method and can be stored as

such.

Main menu:

>XDOS par amet er

>XDOS dosi ng uni t s

>XDOS r e por t s

Submenus:

>XDOS par amet er

selected XDOS type

two of three dosing

parameters will

be shown.

The third parameter will

be automatically

determined by the

Liquino 711 or results

from the dosing itself

and will be printed out in

the result report when

dosing has been con-

cluded.

XDOS t y pe : vol-

volume&time,

time&rate

vol ume 1. 0 mL

f eed rat e ma x mL / mi n

not for volume&time

= selection of volume and dosing time = selection of dosing time and dosing rate

infinite

= continuous dosing; can be ended with <STOP>

max

= highest possible dosing rate (depends on type of

dosing unit.)

cylinder contents. For simple dosing it does not correspond to the effective delivery rate as the filling times of the dosing unit must be taken into ac-

dosi ng t i me 00: 01: 00

not for volume&rate

with <CLEAR>.)

t emp. measur i ng: of f

r ec. i nt er val 00: 01: 00

(only for temp. measuring 'on')

711 Liquino, Instructions for use

4.4 XDOS mode - controlled dosing

78

>XDOS par amet er

Filling rate of dosing unit

max,

= highest possible filling rate (depends on type of dosing

The filling rate is the adjustable piston stroke speed for aspirating the cylin-

>XDOS par amet er

Automatic filling after dosing

on, off

paramet er s

Setting the dosing unit(s)

Navigate with <ENTER>

>XDOS dosi ng uni t s

Use of one or two dosing drives

single,

= dosing with one dosing drive

>XDOS dosi ng uni t s

Dosing drive connection

DOS1, DOS2, DOS3, DOS4

>XDOS dosi ng uni t s

Name of dosing unit used

Selection list

see configuration '>dosi ng uni t s'

>XDOS dosi ng uni t s

Port allocations of dosing unit

default,

= standard port occupancy, see page 76

>XDOS dosi ng uni t s

Dosino port through which dosing is carried

1…4

onl y f or ' c ust om'

>XDOS dosi ng uni t s

Dosino port from which the dosing cylinder is filled.

1…4

onl y f or ' c ust om'

>XDOS dosi ng uni t s wast e port 4

Dosino port for excess reagent with PREP.

1…4

onl y f or ' c ust om'

For tandem dosing the

Maximal values for dosing and filling rates

Cylinder vol. max. rate

2 mL 6.66 mL/min 5 mL 16.66 mL/min 10 mL 33.33 mL/min 20 mL 66.66 mL/min 50 mL 166.66 mL/min

These are pure piston stroke rates; filling times not taken into account.

>XDOS dosi ng uni t s

fill rate ma x mL / mi n

0.001…166.66

unit.)

der contents. Reduce the filling rate for liquids with a higher density or viscosity, as otherwise too rapid filling may cause an underpressure in the cylinder. The time for completely filling an empty dosing cylinder is approx. 20 seconds at max. filling rate (including stopcock switching); at slower filling rates it takes correspondingly longer.

auto fill: on

set up: si ngl e

tandem

= use of two dosing drives for interruption-free dosing

settings for two dosing

drives given alongside

must be carried out.

They are listed one

after another in the

menu.

It is a good idea to use

the same settings for

both dosing drives.

dosi ng dr i v e: DOS 1

dos. uni t : def aul t

por t use: def aul t

custom

dosi ng por t 1

f i l l i ng por t 2

= user-defined port allocation , see below

out.

711 Liquino, Instructions for use

4. Detailed description

79

paramet er s

Monitoring function settings

Navigate with <ENTER>

>XDOS moni t or i ng

Temperature monitoring

>XDOS moni t or i ng

Lower temperature limit

-70…200.0

>XDOS moni t or i ng

Upper temperature limit

-70…200.0

>XDOS moni t or i ng

Reaction if upper or lower temperature limit is infringed

none,

= no reaction (alarm pins still active)

>XDOS moni t or i ng

Definition of the active alarm pins of the remote connection

none,

= no activation

>XDOS moni t or i ng

Volume monitoring function

on, off

>XDOS moni t or i ng crit. volume 10000 mL

Absolute volume limit for terminating dosing

0.0…99999.9

paramet er s

Definition of requests at start of dosing

Navigate with <ENTER>

>XDOS pr esel ect i ons

Automatic request of up to 3 identification texts

id1,

= only ID1 is requested

The alarm pins can be

>XDOS moni t or i ng

t emper at ur e: of f

on, off

l o w l imit - 70 ° C

upper l i mi t 200 ° C

act i on: none

stop,

hold

wait

= dosing is stopped = dosing is interrupted and can be continued with <CONT> = dosing is interrupted and automatically continued as soon as the measuring temperature is again within the limits.

used to switch an external

instrument connected to

the remote socket, e.g. a

heating bath or a

thermostat.

You are recommended to

use Metrohm Relay Box

731.

>XDOS pr esel ect i ons

al ar m pi ns: none

under,

over

vol ume: of f

onl y f or ' vol ume: on'

r eq. i de nt : of f

id1&2,

= Output2 lead (Lower Limit, pin 4) activated when temperature too low = Output1 lead (Upper Limit, pin 18) activated when temperature too high

all

= Output1 and Output2 activated when corresponding temperature limits are infringed (see above)

= ID1 and ID2 are requested

all,

= ID1, ID2 and ID3 are requested

off

= no request

711 Liquino, Instructions for use

Use identification texts (ID1…3) for identifying your sample or your test. The IDs will be printed out in the report of the dosing procedure so that the individual result reports or curves are identified unambiguously.

4.4 XDOS mode - controlled dosing

80

>>XDOS pr ompt s

Display text for requesting the first ID

14 ASCII characters

>>XDOS pr ompt s

Display text for requesting the second ID

14 ASCII characters

>>XDOS pr ompt s

Display text for requesting the third ID

14 ASCII characters

>XDOS pr esel ect i ons

Delay time before dosing

HH:MM:SS

paramet er s

Report definitions for result output

Navigate with <ENTER>

>XDOS r e por t s

Automatic axis scaling for temperature curves

on, off

> XDOS Re po r t s

Lower limit value for temperature axis

>XDOS r epor t s

Upper limit value for temperature axis

-70…200

>XDOS r epor t s no. 1

Selection of one or more reports to be printed out when dosing is completed.

off

= no report

>XDOS r epor t s no. 2

… up to eight reports are possible

…

>XDOS pr esel ect i ons >>XDOS pr ompt s

Submenu for definition of the request texts

i d1 I d1

i d2 I d2

i d3 I d3

st ar t del ay 00: 00: 00

>XDOS r e por t s

t emp. aut o scal e: on

t emp. scal e l ow - 70 ° C

onl y f or aut o scal e ' of f '

t emp. scal e hi gh 200 °C

onl y f or aut o scal e ' of f '

r epor t : of f

-70…200

result,

parameter,

curve,

V-list,

T-list,

comb. list,

= list of relevant results = list of all method parameters = dosing curve, if necessary combined with temperature curve = volume list, list of dosed volumes at events = temperature list, list of measured temperatures = combined volume and temperature list = FORM FEED; triggers page feed at printer

ff

(important for laser and inkjet printers for ejecting pages)

r epor t : of f

Examples of various reports are shown on the following pages.

711 Liquino, Instructions for use

81

Parameter Report

Result Report

4. Detailed description

4.4.2 Examples of reports - XDOS mode

Temperature-controlled dosing with volume and time selection

711 Liquino 0220 711.0011 date 1998-09-30 time 11:51 *** Dev. Dept. *** dm *** Metrohm Ltd mode: XDOS user method: TempDos1 lot no. 12-2 parameters >XDOS parameter XDOS type: volume&time volume 10.0 mL dosing time 00:02:00 temp. measuring: on rec. interval 00:00:10 fill rate max mL/min auto fill: on >XDOS dosing units setup: single dosing drive: DOS1 dos.unit: D3 port use: custom dosing port 1 filling port 2 waste port 1 >XDOS monitoring temperature: on low limit 20.0 °C upper limit 30.0 °C action: wait alarm pins: none volume: off >XDOS preselections req.ident: id1 >>XDOS prompts id1 lot no. id2 id2 id3 id3 start delay 00:00:00 >XDOS reports temp. auto scale: on report1: result report2: curve report3: comb. list report4: off report5: off report6: off report7: off report8: off

------------

711 Liquino 0220 711.0011 date 1998-09-30 time 11:39 *** Dev. Dept. *** dm *** Metrohm Ltd mode: XDOS user method: TempDos1 lot no. 12-2

total dosing time = 000:02:17 total volume = 10.000 mL dosing rate = auto ============

← instrument number and program version ← date and time ← 3-line report header

← mode and method name ← ID1, identification with preselected display text

← dosing parameters

← dosing unit settings

← monitoring function settings

← request settings

← report definitions

← identification of reproduced reports

← see above

← effective time * ← dosed volume ← dosing rate ← identification of original report

* total time including waiting times during infringements of temperature limits or during filling

711 Liquino, Instructions for use

4.4 XDOS mode - controlled dosing

82

Curve Report

Combined List

============

Temperature curve

Temperature limit

Temperature limit reached

Dosing interrupted

711 Liquino 0220 711.0011 date 1998-09-30 time 11:39 *** Dev. Dept. *** dm *** Metrohm Ltd mode: XDOS user method: TempDos1 lot no. 12-2

← volume/temperature curve

============

711 Liquino 0220 711.0011 date 1998-09-30 time 11:39 *** Dev. Dept. *** dm *** Metrohm Ltd mode: XDOS user method: TempDos1 lot no. 12-2

time vol.(mL) temp(°C) event

---------------------------------------000:00:00 0.000 *** START *** 000:00:00 0.000 27.5 000:00:10 0.828 28.5 000:00:20 1.656 29.5 000:00:25 2.075 T-limit,wait 000:00:30 2.075 30.0 upper T-limit 000:00:40 2.075 30.0 upper T-limit 000:00:42 2.075 continue 000:00:50 2.751 29.5 000:01:00 3.584 29.5 000:01:10 4.416 29.5 000:01:20 5.249 29.0 000:01:30 6.081 29.5 000:01:40 6.914 29.5 000:01:50 7.746 29.0 000:02:00 8.579 29.0 000:02:10 9.411 28.5 000:02:17 10.000 *** END *** 000:02:20 28.5 000:02:30 28.5

← tabular list of volumes, temperatures and events

← start of dosing

← temperature limit reached, dosing interrupted

← temperature back in limit, dosing continued

← end of dosing

← procedure ended after dosing unit has been filled.

711 Liquino, Instructions for use

4. Detailed description

83

4.5 SEQ mode - complex processes

The SEQ mode (sequence) of the Liquino allows complex process sequences with a total of up to 75 steps to be created. The individual steps can consist of methods (stored modes) or auxiliary commands. Sequences can be processed several times in automatic operation.

Applications in synthesis For example, in synthesis applications in particular it may be useful to allow several XDOS modes to be carried out one after another and to extend these with time functions and communication commands.

An example: Step 1: wait for time (TIMER command) Step 2: add solvent (XDOS method) Step 3: switch on stirrer (CTRL remote command) Step 4: fill 1st educt into apparatus (XDOS method) Step 5: switch on heating bath (CTRL remote command) Step 6: add 2nd educt drop by drop (XDOS method, temperaturecontrolled) Step 7: wait for reaction (PAUSE command) Step 8: switch off heating bath (CTRL remote command)

Applications in analysis In analysis process sequences are used wherever simple instruments are used to control individual automated systems. The SMPL mode is chiefly used in such applications to carry out sample preparation. In the process sequence various analytical instruments and peripheral units can be started, time-controlled if necessary.

An example:

711 Liquino, Instructions for use

Step 1: Sampling (SMPL method) Step 2: pH/mV measurement (CTRL remote command) Step 3: Titration (SMPL method with start of titration)

Processing a sequence A sequence is a series of part-steps which are carried out one after another. Each step defines a command. The command 'Method' as a special case causes a stored method to be loaded; this consists of a mode (e.g. XDOS, etc.) with its specially defined parameters. The other commands which are available carry out simple functions with one or two parameters. A sequence can be processed several times without interruption. The parameter 'auto start' determines the number of times it is carried out.

4.5 SEQ mode - complex processes

84

>SEQ sequence

The process sequence is defined in the parameter menu and is part of the method. The individual steps can be programmed in sequence. It is possible to insert steps in the sequence at a later date (<INSERT> key) or to delete whole steps from the sequence (<DELETE> key). Example:

aut o st ar t 3 st ep 1 command: TI MER dat e 1998- 12- 01 t i me 10: 00: 00 st ep 2 command: METHOD met hod: XDOS1 st ep 3 command: CONTROL i nt er f ace: Remot e pat t er n 0001---st ep 4 command: PAUSE pause 00: 01: 00 st ep 5 c ommand: CONTROL i nt er f ace: Remot e pat t er n 0000---st ep 6 command: SCAN i nt er f ace: Remot e pat t er n 00001--...

4.5.1 Commands

Sub-methods Any number of methods can be used in a sequence, with the exception of GLP methods or methods which themselves represent a sequence. A precondition is that they are stored either in the internal memory (<USER METH> key) or on an inserted memory card (<MEM CARD> key). Avoid storing methods under the same name in the internal memory and on the memory card if the card is always inserted in the instrument. The Liquino will always load the version of the method which is stored in the internal memory. If you work with memory cards you must take the following points into consideration. Various directories can be created on a card. When a sequence is being processed the Liquino will only access the directory which is currently opened. Before you use a sequence in which a method is stored on a memory card you must select the corresponding directory. This is done by pressing the <MEM CARD> key and then pressing the <> key three times. If '>change di r ect or y' is now shown, press <ENTER> and use the <SELECT> key to select the required directory. Confirm your selection with <ENTER>. See also page 128ff.

 3 repeats of the sequence

 start at a particular time

 carry out method (XDOS1)

 start determination

 minimum waiting period

 reset remote leads

 wait for end of determination

711 Liquino, Instructions for use

4. Detailed description

85

Line conditions:

Auxiliary and communication commands Time-oriented auxiliary commands and communication commands are available.

• PAUSE — this command interrupts sequence processing for a de-

fined period.

• TIMER — sequence processing is interrupted until a defined time

(date and time) has been reached.

• CONTROL — during the sequence processing it is possible to set a

particular signal pattern at a remote connection or to send a character string via an RS232 connection to a connected instrument. The corresponding instrument interface can be selected.

Remote connection: Four of the eight output lines (Output4…7) of the remote socket can be set. The lines Output0 to Output3 are reserved for functions of the various instrument modes. A bit pattern is selected which gives the conditions of the output lines (e.g. the status of the 'External start' line which is used to start a Metrohm instrument). Each bit corresponds to an output line.

Output 7 6 5 4 3 2 1 0 Bit 7 6 5 4 3 2 1 0

(Bits are always numbered from right to left)

Example:

i nt er f ace: Remot e pat t er n 0100---- (lines 0…3 are reserved)

command: CONTROL

0 = inactive (high) 1 = active (low) * = as chosen

711 Liquino, Instructions for use

This example sets output line 6 active (1=set). This line starts a Titrino, provided that remote cable 6.2141.090 is used to make the connection. Output line 6 of the Liquino is connected to input line 0 of the Titrino and starts a determination when it is activated.

Output lines which are of no interest should be masked with an asterisk (*).

With a suitable multiple cable (with special wiring) it is possible to control several instruments simultaneously via the remote leads. The bit patterns for the CONTROL command can be combined, i.e. 2 Titrinos can be started simultaneously and the end of both determinations can be scanned with a SCAN command.

Details about the remote interface can be found under 'Remote Control Reference'.

4.5 SEQ mode - complex processes

86

Line conditions:

RS232 connection: Data (=character strings) can be sent to connected instruments via the serial RS interface.

Make sure that the transmission parameters of the RS232 interface agree with those of the connected instrument (see configuration menu >RS232 Settings, page 21).

Any combination of letters, numbers and special characters can be selected from the Liquino character set. To enter letters and special characters press the <ALPHA> key, see also page 66.

This function is particularly suitable for instruments with the Metrohm remote control language. Metrohm instruments 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;$H Hold, interrupt determination &M;$C Continue, restart determination

Details about the Metrohm remote control language can be found in the ’Instructions for use’ of the corresponding instrument.

• SCAN — this command has the effect of stopping the sequence. In

order to continue the sequence a particular signal pattern at a remote connection or the receipt of a defined character string via an RS232 connection is necessary. The corresponding instrument interface can be selected.

Remote connection: Eight input lines are available for communication with external instruments. Five of these (Input3…7) can be scanned with the SCAN command. Lines Input0 to Input2 are reserved for the functions START, STOP and HOLD/CONTINUE. The condition of the input lines (e.g. the status of the ready line to scan for the titration end at the Titrino) is compared with a preselected bit pattern. Each bit corresponds to an input line.

Input 7 6 5 4 3 2 1 0 Bit 7 6 5 4 3 2 1 0

(Bits are always numbered from right to left)

command: SCAN

0 = inactive (high) 1 = active (low) * = as chosen

Example:

i nt er f ace: Remot e pattern 0***1--- (lines 0…2 are reserved)

The above command expects an active input line 3 (1=set). This line is set, e.g. by a Titrino, after a titration has been ended and the Titrino can again accept a start signal. A precondition is that the remote cable 6.2141.090 is used.

711 Liquino, Instructions for use

4. Detailed description

87

Input lines which are of no interest or for which no defined condition can be predicted should be masked with an asterisk (*).

With a suitable multiple cable (with special wiring) it is possible to scan several instruments simultaneously via the remote lines. The bit patterns for the SCAN command can be combined, i.e. 2 Titrinos can be monitored simultaneously and the end of both determinations can be scanned. Please note that several instruments (Titroprocessors, 691 pH meter) only send short impulses at the end of a determination (typically 200 ms) and therefore for these instruments a combined scan of the end of the determination together with other instruments is only possible under certain (time-related) conditions. Details about the remote interface can be found under 'Remote Control Reference'.

RS232 connection: When scanning the RS232 connection the input buffer of the interface is monitored. Incoming data are compared with the selected character string. The lines received must be concluded with the ASCII characters CR and LF. Incoming data are checked character by character. Any combination of letters, numbers and special characters from the 711 Liquino character set can be selected. To enter letters and special characters press <ALPHA> key, see also page 66. ‘*' can be used as place holder for any character strings. (If '*' is interpreted as an ASCII character then '**' must be used). A place holder can be set within a character string. When the first part of the character string has been recognized correctly then the first appearance of the character which stands after the '*' is searched for. The comparison of the second part of the character string is carried out.

This function is particularly suitable for instruments with the Metrohm remote control language. The AutoInfo status messages can be scanned. The most useful of these are:

*.T.R" Ready, 'Ready' condition is reached, e.g. after titration *.T.F" Final, end of determination is reached *.T.S" Stop, instrument stopped manually *.T.G" Go, instrument starts *.E;* Error, error message

711 Liquino, Instructions for use

4.5 SEQ mode - complex processes

88

These status messages are only transmitted if first the corresponding status message has been switched on, e.g. for a Titrino with the command:

command: CONTROL i nt er f ace: RS s t r i n g : &Se . A. T . R" ON"

Details about the Metrohm remote control language can be found in the ‘Instructions for use’ of the corresponding instrument.

It is essential that the transmission parameters of the RS232 interfaces of both instruments are in agreement. Use RS cable

6.2125.010 for the connection.

• ENDSEQ — this command is used for marking the end within a se-

quence. It can be inserted into any command line for test purposes. This always has the effect that the sequence is only processed up to this line. However, it is not essential that a sequence has an end marking.

SEQ as method A process sequence can, like the other instrument modes, be stored as a method. Sub-methods must be defined and stored before a sequence is put together.

Before carrying out a SEQ method make sure that all the sub-methods required are available, i.e. that they have not been deleted.

711 Liquino, Instructions for use

4. Detailed description

89

paramet er s >SEQ sequence

Open submenu with <ENTER>

paramet er s

Use <HOME> or <END> to jump to first or last menu point Return to basic condition with <QUIT>

paramet er s

Process sequence

Navigate with <ENTER>

>SEQ sequence

Number of times sequence is to be repeated (confirm with <ENTER>)

1…99999,

>SEQ sequence st ep 1

Define step 1 (Select command with <SELECT>)

METHOD, PAUSE, TIMER,

Parameters of the individual commands can be

>SEQ sequence st ep 75

Further steps, up to step 75

METHOD, PAUSE, TIMER,

Parameters of the individual commands can be

Up to 75 commands can be programmed in the sequence. Each

4.5.2 SEQ mode parameters

B

PARAM

All settings in the parameter menu form a method and can be stored as

such.

Main menu:

>SEQ pr esel ect i ons

Submenus:

>SEQ sequence

aut o st ar t 1

Use <> or <> to move down or up from one menu point to the

infinite

(can be set with the <CLEAR> key)

command: NO OP E RAT I ON

SCAN, CONTROL, ENDSEQ,

NO OPERATION

command: NO OPERATI ON

defined after confirmation with <ENTER>.

…

SCAN, CONTROL, ENDSEQ,

command forms a small submenu. After confirming the parameters of the individual commands a new step is automatically attached to the sequence.

In the sequence (step 1… x) quick navigation is possible by using the cursor keys <> and <>. The <HOME> and <END> keys allow a jump to the start or finish of the sequence.

With the <INSERT> key a new step can be inserted before the selected command. <DELETE> deletes the selected command from the sequence. The following steps move up automatically.

711 Liquino, Instructions for use

NO OPERATION.

defined after confirmation with <ENTER>.

4.5 SEQ mode - complex processes

90

paramet er s

Definition of requests at start of sequence

Navigate with <ENTER>

>SEQ pr esel ect i ons

Automatic request for up to 3 identification texts

id1,

= only ID1 is requested

>>SEQ pr ompt s

Display text for requesting the first ID

8 ASCII characters

>>SEQ pr ompt s

Display text for requesting the second ID

8 ASCII characters

>>SEQ pr ompt s

Display text for requesting the third ID

8 ASCII characters

that the individual reports are identified unambiguously.

paramet er s

Report definitions for result output

Navigate with <ENTER>

>SEQ r epor t s no. 1

Selection of one or more reports to be printed out when the process is completed.

off

= no report

>SEQ r epor t s no. 2

… up to two reports are possible

…

>SEQ pr esel ect i ons

r eq. i de nt : of f

id1&2,

= ID1 and ID2 are requested

all,

= ID1, ID2 and ID3 are requested

off

= no request

>SEQ pr esel ect i ons >>SEQ pr ompt s

Submenu for definition of the request texts

i d1 I d1

i d2 I d2

i d3 I d3

Use the identification texts (ID1…3) for identifying your sample or your test. The IDs will be printed out in the report of the dosing procedure so

>SEQ r e por t s

r epor t : of f

parameter,

r epor t : of f

= list of all SEQ parameters

ff

= FORM FEED; triggers page feed at printer (important for laser and inkjet printers, for ejecting pages)

711 Liquino, Instructions for use

4. Detailed description

91

METHOD

>SEQ sequence st ep x

Carry out sub-method

Edit parameters with <ENTER>

>SEQ sequence st ep x

Name of method

Select,

<SELECT> can be used to select a method

PAUSE

>SEQ sequence st ep x

Sequence interruption

Edit parameters with <ENTER>

>SEQ sequence st ep x

Definition of pause period

HH:MM:SS

<CLEAR> can be used to delete the entry.

TIMER

>SEQ sequence st ep x command: TI MER

Time when sequence is to be continued

Edit parameters with <ENTER>

>SEQ sequence st ep x

Date

YYYY-MM-DD

<CLEAR> can be used to delete the entry.

>SEQ sequence st ep x

Time

HH:MM:SS

<CLEAR> can be used to delete the entry.

SCAN

>SEQ sequence st ep x

Scan interface

Edit parameters with <ENTER>

>SEQ sequence st ep x

Selection of interface

Remote

= monitor remote socket

4.5.3 Commands in a sequence

command: ME T H OD

met hod:

command: PAUSE

pause 00: 00: 00

dat e 1998- 01- 01

8 ASCII characters

stored in the internal memory or on a memory card.

711 Liquino, Instructions for use

t i me 12: 00: 00

command: SCAN

The sequence is stopped while the command is carried out.

i nt er f ace: R e mo t e

RS

= monitor RS232 interface

4.5 SEQ mode - complex processes

92

>SEQ sequence st ep x

Bit pattern of input lines of the remote socket

00000---…11111---

>SEQ sequence st ep x

Character string in input buffer of serial RS232 interface

15 ASCII characters

CONTROL

>SEQ sequence st ep x

Operate interface

Edit parameters with <ENTER>

>SEQ sequence st ep x

Select interface with

Remote

= output lines of remote socket

>SEQ sequence st ep x

Bit pattern for setting output lines of remote socket

0000----…1111----

>SEQ sequence st ep x

Character string which is to be sent via the RS232 interface

15 ASCII characters

ENDSEQ

>SEQ sequence st ep x

End mark of the sequence

This command can be used for marking the end

1 = line active (low level) 0 = line inactive (high level) * = condition will not be tested

pat t er n *****---

only for 'interface: Remote'

st r i ng

<CLEAR> can be used to delete the entry.

1 = line active (low level) 0 = line inactive (high level) * = condition will not be changed

only for 'interface: RS'

Input in text input mode. Press <ALPHA> key.

command: CONTROL

i nt er f ace: R e mo t e

pattern ****----

only for 'interface: Remote'

st r i ng

<CLEAR> can be used to delete the entry.

RS

= send data via RS232 interface

<CLEAR> can be used to delete the entry.

Input in text input mode. Press <ALPHA> key.

comma nd: ENDSEQ

only for 'interface: RS'

within a sequence. It is therefore very useful for testing long sequences. It is not necessary to set an ENDSEQ mark at the end of a sequence.

<CLEAR> can be used to delete the entry.

711 Liquino, Instructions for use

93

Parameter-Report

4. Detailed description

4.5.4 Example of a report - SEQ mode

Sequences

711 Li qui no 0220 711. 0011 dat e 1998- 10- 20 t i me 14: 36 * * * Dev. Dept . *** dm * * * Met r ohm Lt d mode: SEQ user met hod: SEQ1 l ot no. 12- 1 pr oj ect no. 4. 567. 98 par amet er s >SEQ s equence aut o st ar t 1 st ep 1 command: TI MER dat e 1998- 12- 01 t i me 10: 00: 00 st ep 2 command: METHOD met hod: XDOS1 st ep 3 command: CONTROL i nt er f ace: Remot e pat t er n 0001---st ep 4 command: PAUSE pause 00: 01: 00 st ep 5 c ommand: SCAN i nt er f ace: Remot e pat t er n 00001--st ep 6 command: NO OPERATI ON >SEQ pr esel ect i ons r eq. i dent : i d1&2 >>XDOS pr ompt s i d1 l ot no. i d2 pr oj ect no. i d3 I d3

>SEQ r epor t s r epor t 1: of f r epor t 2: of f

------------

← instrument number and program version ← date and time ← 3-line report header

← mode and method name ← ID-texts and entries

← definition of process sequence ← number of repeats

← start at a certain time

← sub-method with XDOS mode

← start external instrument

← delay period

← wait for end of determination

← end of sequence

← request settings

← report definitions

← identification for reproduced reports

711 Liquino, Instructions for use

4.6 CONT mode - preparation of solutions

94

4

2

1

3

Port allocation

the keyboard.

Mass unit

Type of calculation

mol/L

molar fraction concentration

g/L

mass concentration

% (percent by weight)

mass fraction

4.6 CONT mode - preparation of solutions

The CONT mode (content) allows the comfortable preparation of solutions or dilutions. With the 711 Liquino the required concentration of the solution can be set precisely. Various dosing procedures are available.

The port allocation of the Dosino in the CONT mode is defined as follows:

Port 1 Dosing port Port 2 Filling port (with dipper tube) Port 3 empty Port 4 Waste (for PREP function)

The port allocation cannot be altered via

4.6.1 Preparation of solutions

If a 711 Liquino is used it is not necessary to weigh out the required amount of a substance with total accuracy. In the CONT mode the Liquino automatically calculates the required volume of solvent needed to obtain the necessary concentration with the sample weight used, e.g. for a standard solution. A balance can be connected directly to the 711 Liquino via an RS232 cable so that the preparation of standard solutions can be automated to a large extent. There is the possibility of documenting the dosing by printing out a result report. The simultaneous connection of a balance and a printer is possible (with branch plug 6.2125.030 and cable 6.2125.010).

Depending on the unit of mass of the target concentration the following dosing procedures can be used for the preparation of solutions:

The necessary information can be stored as a method. These are:

− target content (in mol/L, g/L or %)

− target volume in mL

− factor (e.g. relative content of original substance in g/g)

− molar mass (only for molar fraction concentration)

− density of solvent in g/mL (only for mass fraction)

It is assumed that the Dosino with dosing unit is mounted on a solvent bottle.

711 Liquino, Instructions for use

Metrohm 711 User Manual

Specifications and Main Features

Frequently Asked Questions

User Manual