Metrohm 833IC User Manual

Download

833 IC Liquid Handling Unit

CH-9101 Herisau/Switzerland E-Mail info@metrohm.com Internet www.metrohm.com

Instructions for Use

8.833.1003

CH-9101 Herisau/Switzerland E-Mail info@metrohm.com Internet www.metrohm.com

833 IC Liquid Handling Unit

Instructions for Use

8.833.1003 10.2003 / pkl

Teachware Metrohm AG Oberdorfstrasse 68 CH-9101 Herisau

teachware@metrohm.com

1st Edition 2003

Although all the information given in these instructions has been checked with great care, errors cannot be entirely excluded. Should you notice any mistakes please inform the author at the address given above.

Table of contents

1 Introduction ................................................................ 1

1.1 Instrument description ................................................................................1

1.1.1 833 IC Liquid Handling Pump Unit..................................................................... 1

1.1.2 833 IC Liquid Handling Suppressor Unit ........................................................... 2

1.1.3 833 IC Liquid Handling Sample Preparation Unit.............................................. 3

1.1.4 833 IC Liquid Handling Dialysis Unit.................................................................. 4

1.1.5 833 IC Liquid Handling Ultrafiltration Unit.......................................................... 5

1.2 Parts and controls .......................................................................................6

1.3 Information about these Instructions for Use ............................................8

1.3.1 Arrangement....................................................................................................... 8

1.3.2 Notation and pictograms.................................................................................... 9

1.4 Safety information .....................................................................................10

1.4.1 Electrical safety................................................................................................. 10

1.4.2 General safety rules.......................................................................................... 10

2 Installation ............................................................... 11

2.1 Instrument setup .......................................................................................11

2.1.1 Packaging......................................................................................................... 11

2.1.2 Checks.............................................................................................................. 11

2.1.3 Location ............................................................................................................ 11

2.1.4 Arranging the instruments ................................................................................ 11

2.2 Mains connection ......................................................................................12

2.2.1 Setting the mains voltage................................................................................. 12

2.2.2 Fuses ................................................................................................................ 13

2.2.3 Mains cable ...................................................................................................... 13

2.2.4 Switching the instrument on/off........................................................................ 13

3 Basic instrument ...................................................... 14

3.1 Electrical connection.................................................................................14

3.1.1 Connecting to 761 Compact IC ....................................................................... 14

3.1.2 Connecting to 819 IC Detector......................................................................... 16

3.1.3 Connecting to 830 IC Interface ........................................................................ 18

3.2 Assembly the pump tubing .......................................................................19

3.3 Operation ...................................................................................................23

3.3.1 Switching the instrument on/off........................................................................ 23

3.3.2 Program settings .............................................................................................. 23

4 833 IC Liquid Handling Pump Unit........................... 27

4.1 Connection of the suppressor module ....................................................27

5 833 IC Liquid Handling Suppressor Unit ................. 31

5.1 Connection of the Suppressor module ....................................................31

5.2 Handling the suppressor module .............................................................35

6 833 IC Liquid Handling Sample Preparation Unit ... 36

6.1 Connection to modular IC system for neutralization .............................36

6.1.1 Electrical connections ...................................................................................... 37

6.1.2 Connection of the sample preparation module ............................................... 38

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

Table of contents

6.2 Connection to modular IC system for cation separation ........................43

6.2.2 Settings in IC Net.............................................................................................. 47

6.3 Handling the sample preparation module................................................49

7 833 IC Liquid Handling Dialysis Unit .......................50

7.1 Flow diagram for dialysis..........................................................................51

7.2 Electrical connection.................................................................................52

7.2.1 Dialysis without suppression............................................................................ 52

7.2.2 Dialysis with suppression................................................................................. 53

7.3 Settings in IC Net.......................................................................................54

7.3.1 Dialysis without suppression............................................................................ 54

7.3.2 Dialysis with suppression................................................................................. 55

7.4 Assembling the dialysis cell .....................................................................56

7.5 Making the capillary connections.............................................................57

7.5.1 Preparing the 820 IC Separation Center.......................................................... 57

7.5.2 Connection of the dialysis cell ......................................................................... 58

7.6 Optimizing the dialysis..............................................................................63

7.6.1 Determining the rinsing time ............................................................................ 63

7.6.2 Determining the transfer time........................................................................... 63

7.6.3 Determining the dialysis time........................................................................... 64

7.7 Dialysis procedure ....................................................................................66

8 833 IC Liquid Handling Ultrafiltration Unit.............. 68

8.2 Assembling the ultrafiltration cell.............................................................69

8.3 Connect filtration cell ................................................................................70

8.4 Filtration .....................................................................................................74

8.4.1 Selection of possible sample types ................................................................. 74

8.4.2 Filter working life............................................................................................... 74

8.4.3 Filter membrane selection................................................................................ 75

9 Troubleshooting - maintenance............................... 76

9.1 Faults and their remedies .........................................................................76

9.2 Care and maintenance ..............................................................................79

9.2.1 Instrument care ................................................................................................ 79

9.2.2 Maintenance by Metrohm service.................................................................... 79

9.2.3 Shut down ........................................................................................................ 79

9.2.4 Replacing the pump tubing ............................................................................. 80

9.2.5 Changing the filter ............................................................................................ 81

9.2.6 Suppressor module / Sample preparation module ......................................... 82

9.2.7 Dialysis cell....................................................................................................... 88

9.2.8 Ultrafiltration cell ............................................................................................... 90

10 Appendix ................................................................... 91

10.1 Technical data............................................................................................91

10.1.1 Basic instrument: 833 IC Liquid Handling Unit 1.833.0010............................. 91

10.1.2 6.2729.100 Dialysis cell.................................................................................... 94

10.1.3 6.2729.110 Ultrafiltration cell............................................................................ 94

10.2 Standard equipment ..................................................................................95

10.2.1 833 IC Liquid Handling Pump Unit .................................................................. 95

10.2.2 833 IC Liquid Handling Suppressor Unit ......................................................... 96

10.2.3 833 IC Liquid Handling Sample Preparation Unit............................................ 97

10.2.4 833 IC Liquid Handling Dialysis Unit ............................................................... 98

10.2.5 833 IC Liquid Handling Ultrafiltration Unit...................................................... 100

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

Table of contents

10.3 Optional accessories ..............................................................................103

10.3.1 Connection cables ......................................................................................... 103

10.3.2 Pumps............................................................................................................. 104

10.3.3 Modules .......................................................................................................... 106

10.4 Validation / GLP .......................................................................................107

10.5 Warranty and Conformity ........................................................................108

10.5.1 Warranty.......................................................................................................... 108

10.5.2 Declaration of Conformity............................................................................... 109

10.5.3 Quality Management Principles ..................................................................... 110

10.6 Index .....................................................................................................111

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

III

Table of contents

List of figures

Fig. 1: Front panel of 833 IC Liquid Handling Unit ............................................... 6

Fig. 2: Rear panelof 833 IC Liquid Handling Unit................................................. 7

Fig. 3: Setting the mains voltage........................................................................ 13

Fig. 4: Connecting the 833 IC Liquid Handling Unit to 761 Compact IC ........... 14

Fig. 5: Connecting the 833 IC Liquid Handling Unit to 819 IC Detector............. 16

Fig. 6: Connecting the 833 IC Liquid Handling Unit to 830 IC Interface ............ 18

Fig. 7: Assembly the pump tubing ..................................................................... 19

Fig. 8: Connections to suppressor module of 820 Separation Center............... 27

Fig. 9: Suppressor module 1.753.0100 .............................................................. 31

Fig. 10: Suppressor module connections for

833 IC Liquid Handling Suppressor Unit................................................. 32

Fig. 11: 1.793.0110 Sample Preparation Module................................................. 36

Fig. 12: Electrical connections for 833 IC Liquid Handling Sample

Preparation Unit and modular IC system for neutralization..................... 37

Fig. 13: Connections at sample preparation module of

the 833 IC Liquid Handling Sample Preparation Unit.............................. 39

Fig. 14: Connection of 833 IC Liquid Handling Sample Preparation Unit

to modular IC system for cation separation ............................................ 44

Fig. 15: 6.2729.100 Dialysis Cell .......................................................................... 50

Fig. 16: Connecting the 833 IC Liquid Handling Dialysis Unit

to a modular dialysis system without suppression ................................. 52

Fig. 17: Connecting the 833 IC Liquid Handling Dialysis Unit

to a modular dialysis system with suppression....................................... 53

Fig. 18: Time program for dialysis without suppression ...................................... 54

Fig. 19: Time program for dialysis with suppression............................................ 55

Fig. 20 Inserting the dialysis cell in the holder..................................................... 57

Fig. 21: Tubing connection system ...................................................................... 58

Fig. 22: 6.2729.110 Ultrafiltration cell ................................................................... 68

Fig. 23 Inserting the ultrafiltration cell in the holder ............................................. 70

Fig. 24: Tubing connection system ...................................................................... 71

Fig. 25: Filter unit PEEK 6.2821.120 ..................................................................... 81

Fig. 26: Actuator assembly................................................................................... 84

Fig. 27: Adjusting the actuator step ..................................................................... 88

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

1.1 Instrument description

1 Introduction

1.1 Instrument description

Within the modular Advanced IC Systems the 833 IC Liquid Handling Unit is the universal building block for the preliminary preparation and

post-treatment of samples and for transporting auxiliary and rinsing solutions. It is available in 5 versions that are matched to the most frequently required applications:

• 2.833.0010 833 IC Liquid Handling Pump Unit

• 2.833.0020 833 IC Liquid Handling Suppressor Unit

• 2.833.0030 833 IC Liquid Handling Sample Preparation Unit

• 2.833.0040 833 IC Liquid Handling Dialysis Unit

• 2.833.0050 833 IC Liquid Handling Ultrafiltration Unit

1.1.1 833 IC Liquid Handling Pump Unit

The 833 IC Liquid Handling Pump Unit corresponds to the basic instrument. It has a 2-channel peristaltic pump and can be included in a modular Metrohm IC system via a remote interface and remotely controlled by the IC Net software.

It can transport two solutions simultaneously and is particularly suitable for the operation of the suppressor module in the 2.820.0230 IC Separation Center for supplying regeneration and rinsing solution.

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

1 Introduction

1.1.2 833 IC Liquid Handling Suppressor Unit

As well as the basic instrument, the 833 IC Liquid Handling Suppressor Unit includes a suppressor module connected to the

basic instrument and also remotely controlled by IC Net.

With the suppressor included in the suppressor module analyses by ion chromatography with chemical suppression can be carried out. The suppressor consists of a total of 3 suppressor units which are used in rotation for suppression, regeneration with sulfuric acid and rinsing with water. In order that each new chromatogram is recorded under comparable conditions a freshly regenerated suppressor unit is normally used. Switching takes place automatically.

The 833 IC Liquid Handling Suppressor Unit is particularly suitable for retrofitting existing IC systems for chemical suppression in a simple way. For example, this means that the 833 IC Liquid Handling Suppressor Unit can be used together with two 819 IC Detectors, two 818 IC Pumps and an 820 IC Separation Center without suppressor (2.820.0220) to realize a complete 2-channel IC system with only a single Separation Center.

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

1.1 Instrument description

1.1.3 833 IC Liquid Handling Sample Preparation Unit

As well as the basic instrument, the 833 IC Liquid Handling Unit includes a reactor block (sample preparation module) that is connected to the basic instrument and also remotely controlled by IC Net.

With the cation exchanger built-into the sample preparation module such inline sample preparation steps as neutralization and cation separation can be carried out for analyses by ion chromatography. The sample preparation module contains a total of three units which are used in rotation for cation exchange, regenerated with acid and rinsed with water. In order that each new chromatogram is recorded under comparable conditions a freshly regenerated cation exchanger is normally used. Switching takes place either automatically by the IC system or manually. As sulfate could interfere with the subsequent IC analysis, the cation exchanger of the sample preparation module usually uses perchloric acid (HClO regeneration.

) instead of sulfuric acid (H2SO4) for

The 833 IC Liquid Handling Sample Preparation Unit is particularly suitable for retrofitting a modular IC system for anion analysis for sample preparation in a simple way. Two typical applications (neutralization: exchange of e.g. Na exchange of e.g. heavy metals for H Instructions for Use. Although the cation exchange technique used is comparable with the principle of suppression of the 833 IC Liquid Handling Suppressor Unit, the 833 IC Liquid Handling Sample Preparation Unit is not suitable for chemical suppression after the separation of anions by ion chromatography.

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

for H+ and cation separation:

) are described in detail in the

1 Introduction

1.1.4 833 IC Liquid Handling Dialysis Unit

As well as the basic instrument, the IC Liquid Handling Dialysis Unit 833 includes a dialysis cell upstream from the sample injector.

The 833 IC Liquid Handling Dialysis Unit is used for online sample preparation in ion chromatography and allows the use of automatic sample dialysis immediately before sample injection. As well as the 2channel peristaltic pump of the basic instrument for transferring the sample and acceptor solution from the dialysis cell itself, the ions from the flowing sample solution are enriched in the stationary acceptor solution and then injected directly into the IC system. As a result of this special stopped flow technique, for which an application for a patent has been made by Metrohm, 100% sample concentration can be achieved in the acceptor solution and in this way it is possible to carry out calibration with external standards in a very easy manner.

The operation of the 833 IC Liquid Handling Dialysis Unit requires the use of an 820 IC Separation Center with one injector and an additional 833 IC Liquid Handling Pump Unit for the sample tramsport. These systems, which are described in the Instructions for Use, require the following instruments:

Operation without

2.819.0110 IC Detector

2.820.0210 IC Separation Center

2.818.0110 IC Pump

2.833.0040 IC Liquid Handling Dialysis Unit

2.833.0010 IC Liquid Handling Pump Unit

suppressor

Operation with suppressor

2.819.0110 IC Detector

2.820.0230 IC Separation Center

2.818.0110 IC Pump

2.833.0040 IC Liquid Handling Dialysis Unit

2.833.0010 IC Liquid Handling Pump Unit (2 x)

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

1.1 Instrument description

1.1.5 833 IC Liquid Handling Ultrafiltration Unit

As well as the basic instrument, the IC Liquid Handling Ultrafiltration Unit 833 includes a filtration cell upstream from the sample injector.

The 833 IC Liquid Handling Ultrafiltration Unit is an instrument for online sample preparation in ion chromatography that allows the inline filtration of the sample immediately before it is injected.

The 833 IC Liquid Handling Ultrafiltration Unit is designed for the filtration of difficult samples that place special demands on the filtration effects and sample throughput.

Of course, all versions of the 833 IC Liquid Handling Unit can also be used with any other commercially available HPLC components.

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

1 Introduction

1.2 Parts and controls

In this section you will find the numbers and names of the parts and controls of the 833 IC Liquid Handling Unit. The numbering is valid for the whole of these Instructions for Use, i.e. bold numbers in the text (e.g.

) refer to the parts and controls shown here.

Fig. 1: Front panel of 833 IC Liquid Handling Unit

Mains lamp

Lights up when instrument is switched on

Holding pin

For inserting the tubing cassettes

32 4 5 6

Contact lever

For controlling the contact pressure

Holding clip

For clicking the tubing cassette in place

Pump drive

Roller head with contact rollers

Tubing cassette

For 6.1826.0X0 Pump tubing

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

Spring lever

For releasing the tubing cassette

1.2 Parts and controls

Fig. 2: Rear panelof 833 IC Liquid Handling Unit

Mains switch

Switch for switching instrument on/off:

I = ON 0 = OFF

12 13 14

Module

Connection for suppressor module and sample preparation module

Mains connection

Mains connection: see Section 2.2

Serial number

Fuse holder

Changing the fuses: see Section 2.2.2.

Step adjustment

Adjusts the actuator rotor

REMOTE actuator

Remote interface for actuator Connection to 761 Compact IC, 819 IC Detector or 830 IC Interface

REMOTE pump

Remote interface for pump Connection to 761 Compact IC, 732/819 IC Detector or 762/830 IC Interface

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

1 Introduction

1.3 Information about these Instructions for Use

Please read through these Instructions for Use carefully before you start to use the 833 IC Liquid Handling Unit. The instructions contain information and warnings that must be observed by the user in order to guarantee the safe use of the instrument.

1.3.1 Arrangement

These 8.833.1003 Instructions for Use for the 833 IC Liquid Handling Unit provide a comprehensive overview of the installation, start-up, operation and technical specifications of this instrument. They are arranged in the following way:

Sect. 1 Introduction

General description of the instrument, numbers and names of the parts and controls, safety information

Sect. 2 Installation

Instrument setup, mains connection

Sect. 3 Basic instrument

Instrument connection, mounting the pump tubing, control via «IC Net»

Sect. 4 833 IC Liquid Handling Pump Unit

Instrument connection

Sect. 5 833 IC Liquid Handling Suppressor Unit

Instrument connection, suppressor module handling

Sect. 6 833 IC Liquid Handling Sample Preparation Unit

Instrument connection to modular system for cation separation and modular system for neutralization, sample preparation module handling

Sect. 7 833 IC Liquid Handling Dialysis Unit

Instrument connection to modular system with manual sample injection, dialysis procedure, dialysis optimization

Sect. 8 833 IC Liquid Handling Ultrafiltration Unit

Instrument connection, general information about filtration

Sect. 9 Troubleshooting -

Troubleshooting and remedies, care and maintenance

Sect. 10 Appendix

Technical data, standard equipment, options, warranty, conformity declarations, index

Please use either the Table of Contents or the Index to find any information you may require.

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

1.3 Information about these Instructions for Use

1.3.2 Notation and pictograms

The following notation and pictograms (symbols) are used in these Instructions for Use:

Pump Menu item, parameter or input

value

in «IC Net» program

SYSTEM STATE Program window

in «IC Net» program

<OK> Button

in «IC Net» program

[ RUN/STOP ] Switch or key

10 Part or control of 833

14 Part or control of 819/820

Danger/Warning This symbol indicates a possible risk of death or injury to the user and possible damage to the instrument or its components by electric current.

Danger/Warning This symbol indicates a possible risk of death or injury to the user and possible damage to the instrument or its components.

Attention This symbol indicates important information that you should read before continuing.

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

Information This symbol indicates additional information and tips which may be of particular use to you.

1 Introduction

1.4 Safety information

1.4.1 Electrical safety

Electrical safety when handling the 833 IC Liquid Handling Unit is guaranteed within the scope of Standard IEC 1010-1 (protection class 1, protection code IP40). The following points must be observed:

• Mains connection

The mains connection must be made in accordance with the instructions given in Section 2.2.

• Opening the instrument

The housing contains no components which could be set or adjusted by the user .

When the 833 IC Liquid Handling Unit is connected to the mains supply the instrument must not be opened, nor should any of its components be dismantled as otherwise you could come into contact with current-carrying components. Before opening the instrument separate it from all current sources and make sure that mains cable

has been removed from mains connection socket

• Protection against electrostatic charges

Electronic components are sensitive to electrostatic charges and can be destroyed by a discharge. Before you touch any electronic components of the 833 IC Liquid Handling Unit you should ground you and your tools by grasping a grounded object (e.g. the instrument housing or a radiator) in order to eliminate any electrostatic charges that may be present.

1.4.2 General safety rules

• Solvent handling

Check the pump tubing and inlet and outlet connections for leaks at regular intervals. Observe the relevant regulations when handling and disposing of flammable and/or toxic solutions.

• Regular replacement of pump tubing

Pump tubing is a consumable and must be replaced from time to time (see Section 9.2.4). Take suitable measures to ensure that any leak in the pump tubing or connections during unattended and continuous operation cannot cause any damage (placing the instrument in a low position, collection trough for escaping liquid).

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

2.1 Instrument setup

2 Installation

2.1 Instrument setup

2.1.1 Packaging

The 833 IC Liquid Handling Unit and its separately packed accessories are supplied in very protective special packaging. These contain impact-absorbing plastic foam linings contained inside a blue plastic film; these are molded to fit the individual components. The instrument itself is contained in a dustproof evacuated polyethylene bag. Please store all this special packaging; it is the only way in which the safe transport of the instrument can be guaranteed.

2.1.2 Checks

Please check that the delivery is complete and undamaged immediately on receipt (compare with delivery note and list of accessories given in Section 10.2). If transport damage is evident please refer to the information given in Section 10.5.1 "Warranty".

2.1.3 Location

Place the instrument on a vibration-free bench in a favorable position for operation and protected from corrosive atmospheres and contamination by chemicals.

2.1.4 Arranging the instruments

Other IC instruments (e.g. 818, 819, 820) can be stacked on top of the 833 IC Liquid Handling Unit. It is best to place it beside the modular IC system or at the bottom of the stack.

The 833 IC Liquid Handling Unit should always be at the bottom so that any leaks which may occur in the pump tubing or connections cannot cause any great damage by escaping liquids (e.g. acids).

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

2 Installation

2.2 Mains connection

Please observe the following rules when connecting the instrument to the electricity supply. If the instrument is operated with an incorrectly set mains voltage and/or an incorrect mains fuse then it represents a fire hazard!

2.2.1 Setting the mains voltage

Before you switch on the 833 Liquid Handling Unit for the first time please check that the mains voltage set on the instrument (see Fig. 3) corresponds to your local mains voltage. If this is not must alter the mains voltage as follows:

1 Pull out mains cable

Remove the mains cable from mains supply connection 9 of the 833 IC Liquid Handling.

the case then you

2 Remove the fuse holder

Use a screwdriver to loosen fuse holder 11 beneath the mains supply connection and remove it completely.

3 Check the fuse

Carefully remove the built-in fuse for the intended voltage from the fuse holder and check its specifications (the position of the fuse in the fuse holder is indicated by the white arrow beside the voltage range):

100…120 V 0.5 A (slow blow) Metrohm No. U.600.0013 220…240 V 0.25 A (slow blow) Metrohm No. U.600.0010

4 Insert fuse

Exchange the fuse if necessary and replace it in the fuse holder.

5 Insert fuse holder

Depending on the required mains voltage, insert the fuse holder in the 833 IC Liquid Handling Unit 833 so that the appropriate voltage range can be read normally and the adjacent white arrow points to the white bar printed beneath the fuse holder (see Fig. 3).

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

2.2 Mains connection

–

Fig. 3: Setting the mains voltage

2.2.2 Fuses

220 –240

100

120

8 Mains switch

9 Mains

connection

220 - 240 V

100 - 120 V

220

240 V

100

120 V

11 Fuse holder

The fuse holder of the 833 IC Liquid Handling Unit contains one of the two fuses 0.5 A/slow blow for 100…120 V or 0.25 A/slow blow for 220…240 V.

Make sure that the instrument is never operated with a different type of fuse as otherwise it represents a fire hazard!

Checking and replacing a fuse is described in Section 2.2.1.

2.2.3 Mains cable

The instrument is supplied with one of the following mains cables:

• 6.2122.020 with SEV 12 plug (Switzerland, …)

• 6.2122.040 with CEE(7), VII plug (Germany, …)

• 6.2133.070 with NEMA 5-15 (USA, …)

which has 3 wires and is fitted with a plug with a grounding pin. If a different plug has to be attached then the yellow/green wire (IEC standard) must be connection to the grounding pin.

Any break in the grounding inside or outside the instrument will make it dangerous!

Insert the mains cable plug in mains connection 9 of the 833 IC Liquid Handling Unit (see Fig. 2).

2.2.4 Switching the instrument on/off

The 833 IC Liquid Handling Unit is switched on and off with mains switch 8 (see Fig. 2). When the instrument is switched on mains lamp 1 lights up.

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

3 Basic instrument

3.1 Electrical connection

Always switch off the 833 IC Liquid Handling Unit and the instrument to which the Liquid Handling Unit is to be connected before you make an electrical connection.

The 833 Liquid Handling Unit can be operated and remotely controlled by a 761 Compact IC, an 819 IC Detector and in a modular system via the 830 IC Interface.

3.1.1 Connecting to 761 Compact IC

Connect the remote connection of the 761 Compact IC with the required remote connections 14 and 15 on the 833 IC Liquid Handling Unit. The peristaltic pump of the Liquid Handling Unit is controlled via remote connection Remote Pump 15, this must always be connected. The connection Remote Actuator 14 is only required for the 833 IC Liquid Handling Suppressor Unit and the 833 IC Liquid Handling Sample Preparation Unit; it is used to switch the suppressor or sample preparation module. The particular modules are connected to the socket Module 13.

761

833

816

Cable

Module

761

833

816

6.2143.200

6.2143.210

Fig. 4: Connecting the 833 IC Liquid Handling Unit to 761 Compact IC

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

3.1 Electrical connection

The following cables are available for these connections:

• 6.2143.200 Cable for one remote connection via

Remote line 1.

To connect a Liquid Handling Unit with a peristaltic pump, e.g.:

2.833.0010 IC Liquid Handling Pump Unit

2.833.0050 IC Liquid Handling Ultrafiltration Unit

• 6.2143.210 Cable for two remote connections via

Remote lines 1 and 2.

To connect a Liquid Handling Unit with a peristaltic pump and a suppressor or sample preparation module, e.g.:

2.833.0020 IC Liquid Handling Suppressor Unit

2.833.0030 IC Liquid Handling Sample Preparation Unit

or To connect two peristaltic pumps, e.g. for dialysis:

2.833.0010 IC Liquid Handling Pump Unit

2.833.0040 IC Liquid Handling Dialysis Unit

• 6.2143.220 Cable for three remote connections via

Remote lines 1, 2 and 4.

To connect up to three Liquid Handling Units, e.g. for dialysis with suppression: 2x 2.833.0010 IC Liquid Handling Pump Unit and 1x 2.833.0040 IC Liquid Handling Dialysis Unit (three peristaltic pumps are switched on and off)

or Ultrafiltration with suppression 1x 2.833.0020 IC Liquid Handling Suppressor Unit and 1x 2.833.0050 IC Liquid Handling Ultrafiltration Unit (two peristaltic pumps are switched on and off and the sample preparation module is switched on)

The remote line via which the control of the Liquid Handling Unit takes place is determined by the wiring of the cable. The active remote line is printed on the 833-end of the cable. This remote line must be set accordingly in the control software «761 Compact IC» or «IC Net», see

Section 4.3.7 In the «761 Compact IC» Instructions for Use and Section

6.5.3 in the «IC Net» Instructions for Use.

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

3 Basic instrument

3.1.2 Connecting to 819 IC Detector

Connect the remote connection of the 819 IC Detector to the necessary remote connections 14 and 15 on the 833 IC Liquid Handling Unit. The peristaltic pump of the Liquid Handling Unit is controlled via remote connection Remote Pump 15, this must always be connected. The connection Remote Actuator 14 is only required for the 833 IC Liquid Handling Suppressor Unit and the 833 IC Liquid Handling Sample Preparation Unit; it is used to switch the suppressor or sample preparation module. The particular modules are connected to the socket Module 13.

819 819

833

816

6.2143.200

Cable

Module

833

816

6.2143.210

Fig. 5: Connecting the 833 IC Liquid Handling Unit to 819 IC Detector

The following cables are available for these connections:

• 6.2143.200 Cable for one remote connection via

Remote line 1.

To connect a Liquid Handling Unit with a peristaltic pump, e.g.:

2.833.0010 IC Liquid Handling Pump Unit

2.833.0050 IC Liquid Handling Ultrafiltration Unit

• 6.2143.210 Cable for two remote connections via

Remote lines 1 and 2.

To connect a Liquid Handling Unit with a peristaltic pump and a suppressor or sample preparation module, e.g.:

2.833.0020 IC Liquid Handling Suppressor Unit

2.833.0030 IC Liquid Handling Sample Preparation Unit

or To connect two peristaltic pumps, e.g. for dialysis:

2.833.0010 IC Liquid Handling Pump Unit

2.833.0040 IC Liquid Handling Dialysis Unit

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

3.1 Electrical connection

• 6.2143.220 Cable for three remote connections via

Remote lines 1, 2 and 4.

Ultrafiltration with suppression 1x 2.833.0020 IC Liquid Handling Suppressor Unit and 1x 2.833.0050 IC Liquid Handling Ultrafiltration Unit (two peristaltic pumps are switched on and off and the sample preparation module is switched on)

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

3 Basic instrument

3.1.3 Connecting to 830 IC Interface

Connect one of the event lines of the 830 IC Interface with one of the required remote connections 14 and 15 on the 833 IC Liquid Handling Unit. The peristaltic pump of the Liquid Handling Unit is controlled via remote connection Remote Pump 15, this must always be connected. The connection Remote Actuator 14 is only required for the 833 IC Liquid Handling Suppressor Unit and the 833 IC Liquid Handling Sample Preparation Unit; it is used to switch the suppressor or sample preparation module. The particular modules are connected to the socket Module 13.

830

833

816

Cable

Module

6.2128.180

830

833

816

6.2128.180

Fig. 6: Connecting the 833 IC Liquid Handling Unit to 830 IC Interface

For each remote connection one 6.2128.180 Cable is required. At the 830 IC Interface 2 × 7 remote connections can be assembled. Which event lines are used for this does not matter; when a system is set up the assignment must only be given correctly in the «IC Net» software when creating a system, see Section 6.1 of the «IC Net» Instructions for

Use.

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

3.2 Assembly the pump tubing

Pump tubing is a consumable whose working life depends on the contact pressure. This is why when the pump is switched off for a long time, the tubing cassette should be lifted by fully loosening spring lever

on the right-hand side (in this way the correctly set optimal

contact pressure is retained).

The 6.1826.0X0 Pump tubing consists of PVC or PP and must therefore not be rinsed with solvents that contain acetone. In this case you should either use different pump tubing or use a different pump for rinsing.

18 17 16 4 519

Tubing cassette

Contact lever

Spring lever

6.1803.0X0 Aspiration

tubeing/capillary

PTFE tubing/capillary, depends on version, see Section 10.2 Standard equipment

20 22 21 20 17

Fig. 7: Assembly the pump tubing

Stopper

The color of the stopper indicates the material and dimensions of the pump tubing, see Tab. 1.

6.2744.160 PEEK Coupling

with tubing security device

6.2821.120 PEEK Filter unit

not contained in all versions, see

Section 10.2 Standard equipment

17 1716

6.2744.010 PEEK compression

fitting

6.2744.034 PEEK coupling

6.1826.0X0 Pump tubing

various tubing is available, depending on the application, see Tab. 1.

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

Discharge capillary

delivery side for connection to: suppressor module sample preparation module dialysis cell ultrafiltration cell

3 Basic instrument

1 Remove tubing cassettes

• Loosen the two tubing cassettes 4 by pressing in spring lever

7 of holding clip 6 and unhinge them from holding pin 2 of

the 833 IC Liquid Handling Unit (see Fig. 1).

2 Insert pump tubing

• Press contact lever 5 on the two tubing cassettes down as far

it will go.

• Insert pump tubing into each tubing cassette as shown in

Fig. 7. Stopper must click into position in the corresponding holder on the left-hand side of the tubing cassette.

3 Attach tubing cassettes

• Hinge the tubing cassettes on holding pin and press down

on the right –hand side until spring lever clicks into position in holding clip 6. Take care that the pump tubing does not kink.

4 Attach coupling to pump tubing

• Attach PEEK coupling 18 to the aspiration end of pump

tubing 19 for both channels (see Fig. 7).

•

Mount PEEK coupling 21 with the tubing security device

(6.2744.160) to the delivery end of pump tubing 19 for both channels. This is done by dismantling the tubing security device and first pushing the sleeve nut and the compression piece onto the tubing.

Attach the tubing to the PEEK coupling and screw the sleeve nut onto the coupling in order to secure the tubing.

5 Mounting of filter unit

• If contained in the standard equipment (see Section 10.2

Standard equipment), screw 6.2821.120 PEEK filter unit 22

onto PEEK coupling 21 (6.2744.160) by using two PEEK compression fittings 17 (6.2744.010) and a piece of aspiration tubing/capillary 16 (6.1803.0X0) at the delivery end of pump tubing 19.

Setting the contact pressure correctly:

Press contact lever 5 until the solutions are just aspirated. Then press the contact lever up by 1 further click to achieve the optimum contact pressure.

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

3.2 Assembly the pump tubing

In addition to the correct contact pressure, the delivery rate of the 833 IC Liquid Handling Unit depends primarily on the inner diameter of pump tubing 19. Different pump tubing can be used depending on the application.

The following table provides information about the properties and use of the available pump tubing.

Tab. 1: Using 6.1826.0X0 Pump tubing

Used with Order no. Description

2.833.0030 IC Liquid Handling Sample Preparation Unit: both channels

6.1826.010 Pump tubing

PVC (Tygon



ST) with 2 permanently

mounted white-white stoppers; i.d. = 1.02 mm ± 0.05 mm, Delivery rate

1.41 mL/min (20 min

1.69 mL/min (24 min

optional 6.1826.020 Pump tubing

PVC (Tygon



ST) with 2 permanently

mounted blue-blue stoppers; i.d. = 1.65 mm ± 0.05 mm, Delivery rate

3.75 mL/min (20 min

4.50 mL/min (24 min

2.833.0040 IC Liquid Handling Dialysis Unit:

channel for supplying acceptor solution

2.833.0050 IC Liquid Handling Ultrafiltration Unit:

channel for transferring filtrate to sample loop

2.833.0040 IC Liquid Handling Dialysis Unit:

channel for supplying sample

6.1826.030 Pump tubing

PVC (Tygon



ST) with 2 permanently

mounted orange-yellow stoppers; i.d. = 0.51 mm ± 0.05 mm, Delivery rate

0.40 mL/min (20 min

0.48 mL/min (24 min

6.1826.040 Pump tubing

PVC (Tygon mounted black-black stoppers; i.d. = 0.76 mm ± 0.05 mm, Delivery rate



ST) with 2 permanently

0.75 mL/min (20 min

0.90 mL/min (24 min

150

-1

)

-1

)

-1

)

-1

)

-1

)

-1

)

-1

)

-1

)

400

150

400

150

400

150

400

2.833.0010 IC Liquid Handling Pump Unit,

2.833.0020 IC Liquid Handling Suppressor Unit: both channels

6.1826.050 Pump tubing

PVC (Tygon mounted white-yellow stoppers; i.d. = 0.57 mm ± 0.05 mm, Delivery rate

0.52 mL/min (24 min

optional 6.1826.060 Pump tubing

PP (PharMed mounted orange-yellow stoppers; i.d. = 0.51 mm ± 0.05 mm, Delivery rate

0.56 mL/min (24 min

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003



ST) with 2 permanently

0.43 mL/min (20 min



) with 2 permanently

0.47 mL/min (20 min

150

-1

)

-1

)

-1

)

-1

)

400

150

400

3 Basic instrument

2.833.0050 IC Liquid Handling Ultrafiltration Unit:

channel for transferring sample to ultrafiltration cell

6.1826.070 Pump tubing

PVC (Tygon



ST) with 2 permanently

mounted yellow-yellow stoppers; i.d. = 1.42 mm ± 0.05 mm, Delivery rate

2.55 mL/min (20 min

3.06 mL/min (24 min

optional 6.1826.110 Pump tubing long-life

PVC (Tygon mounted orange-yellow stoppers; i.d. = 0.51 mm ± 0.0102 mm, Delivery rate



LFL) with 2 permanently

0.40 mL/min (20 min

0.48 mL/min (24 min

optional 6.1826.120 Pump tubing long-life

PVC (Tygon mounted orange-white stoppers; i.d. = 0.59 mm ± 0.05 mm, Delivery rate



LFL) with 2 permanently

0.44 mL/min (20 min

0.53 mL/min (24 min

optional 6.1826.130 Pump tubing long-life

PVC (Tygon mounted white-white stoppers; i.d. = 1.02 mm ± 0.0127 mm, Delivery rate



LFL) with 2 permanently

1.41 mL/min (20 min

1.69 mL/min (24 min

150

-1

)

-1

)

-1

)

-1

)

-1

)

-1

)

-1

)

-1

)

400

150

400

150

400

150

400

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

3.3 Operation

The 833 IC Liquid Handling Unit is operated completely via the Metrohm «IC Net» software.

This Section only described the most important functions and settings for operating the 833 IC Liquid Handling Unit. Further information is given in the Instructions for Use of the «IC Net» and in the online help for the program.

3.3.1 Switching the instrument on/off

Remote control of the 833 IC Liquid Handling Unit by the software requires that the instruments has been installed correctly as described in Section 2.

Switching the instrument on/off

The 833 IC Liquid Handling Unit is switched on and off with mains switch 8 on the rear panel of the instrument (see Fig. 2):

I Instrument switched on 0 Instrument switched off

POWE

When the instrument has been switched on mains lamp 1 lights up to show that it is ready for use.

3.3.2 Program settings

The 833 IC Liquid Handling Unit is operated completely via the Metrohm «IC Net» software.

This section only describes the most important functions and settings for operating the 833 IC Liquid Handling Unit. Further information is given in the Instructions for Use of the «IC Net» and in the online help for the program.

3.3.2.1 833 IC Liquid Handling Unit icon

2.833.00X0 IC Liquid Handling Unit

For differentiating between which version of the 833 is indicated by the instrument icon a tool tip with the name of the corresponding instrument appears when the mouse cursor is placed on the particular icon.

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

3 Basic instrument

3.3.2.2 Settings in the window "833 IC Liquid Handling Unit"

Selection of this menu item with the right-hand mouse key or a doubleclick on the 833 instrument icon opens the window

Unit for parameter settings. It consists of three tabs: Manual, Program

Links.

and

833 IC Liquid Handling

Depending on the version, the title line of the parameter settings window shows

Preparation Unit

833 IC Pump Unit, 833 IC Suppressor Unit, 833 IC Sample

, 833 IC Dialysis Unit or 833 IC Ultrafiltration Unit and (in

brackets) the name of the system folder and the system file.

Manual

The tab

Manual of the window 833 IC Liquid Handling Unit is used for

manually operating the peristaltic pump and the suppressor or sample prep module.

Pump (available with all versions)

<On> Start pump drive. <Off> Stop pump drive.

Suppressor (only available with 833 IC Suppressor Unit)

<Step> Rotate suppressor to the next position. The

time since the last step action is displayed in the field beside the

Actuator (only available with 833 IC Sample Preparation

Unit)

<Step> Rotate sample preparation module to the next

<Step> button.

position. The time since the last step action is displayed in the field beside the

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

<Step> button.

3.3 Operation

Start pump with startup hardware

Automatic start of pump drive with Startup

hardware

Time program

A user-specific time program can be entered on the tab

833 IC Liquid Handling Unit window. Depending on the settings made in

Start mode window (for details see Section 4.4.3 8.110.8281

the

Program in the

Instructions for Use for the Metrodata «IC Net 2.3» software), this

program is started automatically either at the start of the determination (

Start with determination) or when the sample is injected (Start with inject).

Time (1st column) Time at which program instruction is applied.

Entry range:

0.0 ... 999.9 min

If no time is entered, the program instruction is applied together with the last instruction with time entry.

Command (2nd. column) Program instruction (see below). Parameter (3rd column) Parameter for program instruction (see below).

ENABLED Enable program start (a disabled program is

not started).

<Add> Add new program instruction. <Delete> Delete selected program instruction. <Verify> Test the time program (error messages are

displayed if program is wrong).

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

3 Basic instrument

List of program instructions

The following program instructions can be added to the time program on the

Instruction Parameter entry Meaning

Pump on, off Switch on or off the pump drive.

Step Rotate suppressor or sample prep

Program page:

(available for

all versions)

module to the next position. (only available for

Unit and 833 IC Sample Prep Unit)

833 IC Suppressor

Links

Links tab of the 833 IC Pump Unit is used for Event line selection (for

The details see Instructions for Use of «IC Net»).

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

4.1 Connection of the suppressor module

4 833 IC Liquid

Handling Pump Unit

This version is mainly used for supplying a Metrohm Suppressor Module MSM built into a 2.820.0X30 IC Separation Center with

regeneration and rinsing solutions. The Metrohm Suppressor Module MSM is described in detail in Section 2.9.7 of the 819/820 Instructions for Use.

4.1 Connection of the suppressor module

In order to protect the suppressor module against foreign particles an inline filter is mounted between the 833 IC Liquid Handling Unit and the inlet capillary of the suppressor module, see Fig. 7. The most suitable unit is the 6.2821.120 Filter unit PEEK included in the standard equipment.

H2SO4

Waste

The suppressor module is connected to the 833 IC Liquid Handling Pump Unit in accordance with Section 2.9.7 of the 819/820 Instructions for Use. The most important points are described again below, with underlined numbers ## 819/820 Instructions for Use:

Eluent

Waste

referring to the parts and controls in the

Suppressor inlet

capillary for eluent

65 Suppressor inlet

Detector

H2O

capillary for H

66 Suppressor outlet

capillary for H

67 Suppressor outlet

capillary for H

68 Suppressor inlet

capillary for H

69 Suppressor outlet

capillary for eluent

2SO4

Fig. 8: Connections to suppressor module of 820 Separation Center

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

4 833 IC Liquid Handling Pump Unit

1 Connect column to injector

• Remove end caps from column 53.

• without column heating:

Screw inlet end of separating column 53 to column connection capillary 50

(note flow direction)

mounted on the injector.

• with column heating:

Prepare column heating according to Section 2.9.2 of the 819/820 Instructions for Use and screw column connection

capillary 50 compression fitting to injection valve 51

(see Fig. 20, 819/820 Instructions for Use) with a

• With precolumn:

Install precolumn according to the supplied leaflet between inlet of the separating column and the injection valve.

2 Rinse column

• Place a beaker beneath the column outlet.

• Start 818 IC Pump in «IC Net» with suitable flow (see leaflet of

the column) and rinse column for ca. 10 min with eluent.

• Stop 818 IC Pump.

3 Connect column to suppressor module (Suppressor

connection 1)

• Cut inlet capillary 64

module 70

to the required length. Use the 6.2126.080

(marked with "Eluent") of suppressor

Capillary cutter available as an option.

• without column heating

Screw inlet capillary 64 column 53

using a 6.2744.010 compression fitting.

on to the outlet end of separating

• with column heating

Connect capillary 52

at the outlet of the separating column

(see Fig. 20, 819/820 Instructions for Use) to the inlet capillary 64

using the 6.2744.040 Coupling.

4 Fix column

• without column heating

Insert one or two column holders 59 or 6.2027.050) in the mounting rails 58

(6.2027.030, 6.2027.040

and fasten separating

column in the column holder.

• with column heating

Insert column heating according to Fig. 10 (819/820 Instructions for Use) into the Separation Center.

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

4.1 Connection of the suppressor module

5 Connect suppressor module to detector block

(Suppressor connection 1)

• Cut outlet capillary 69

module 70

to the required length. Use the 6.2126.080

(marked with “Detector”) of suppressor

Capillary cutter available as an option.

• Screw outlet capillary 69

on to coupling 71 by using a

6.2744.010 Pressure screw.

• Screw inlet capillary 56

end of coupling 71

of detector block 57 on to the other

6 Mount pump tubing on 833 Pump Unit

• Mount the two lengths of 6.1826.050 Pump tubing (white-

yellow stopper) with aspirating tube 16 and filter unit PEEK

22 6.2821.120 as described in Section 3.2, see Fig. 7.

7 Suppressor connection 2: H2SO4

• Pull inlet capillary 65 (marked with "H2SO4") by hand as far as

required through one of the feedthroughs 14

to the outside

(see Fig. 23 and Fig.24, 819/820 Instructions for Use).

• Screw the filter unit PEEK contained in the standard

equipment of the 833 IC LH Pump Unit on to PEEK coupling 21 (6.2744.160) as described in Section 3.2 at the outlet end of the first piece of pump tubing 19.

• Fasten inlet capillary 65

(23 in Fig. 7) to filter unit PEEK

(6.2821.120) by using a compression fitting 17 (6.2744.010) (see Fig. 7).

• At the inlet end of the first piece of tubing 19 fasten a suitably

long piece of PTFE tubing 16 (6.1803.020) to coupling 18 (6.2744.034) by using a compression fitting 17 (6.2744.010).

• Immerse the other end of the aspiration tubing in a container

with regeneration solution (normally 50 mmol/L H

2SO4

) and fix

it in position.

• Pull outlet capillary 66 of the suppressor module (marked

with "Waste") through opening 18

on the rear panel, lead it

into a sufficiently large waste bottle and fix it in position.

8 Suppressor connection 3: H2O

• Pull inlet capillary 68 (marked with "H2SO4") by hand as far as

required through one of the feedthroughs 14 (see Fig. 23 and Fig.24, 819/820 Instructions for Use).

• Screw the filter unit PEEK contained in the standard

equipment of the 83 IC LH Pump Unit on to PEEK coupling 21 (6.2744.160) as described in Section 3.2 at the outlet end of the second piece of pump tubing 19.

• Fasten inlet capillary 68

(6.2821.120) by using a compression fitting 17 (6.2744.010) (see Fig. 7).

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

to the outside

(23 in Fig. 7) to the filter unit PEEK

4 833 IC Liquid Handling Pump Unit

• At the inlet end of the second piece of tubing 19 fasten a

suitably long piece of PTFE tubing 16 (6.1803.020) to coupling 18 (6.2744.034) by using a compression fitting 17 (6.2744.010).

• Immerse the other end of the aspiration tubing in a container

with rinsing solution (normally dist. H

• Pull outlet capillary 67

of the suppressor module (marked

with "Waste") through opening 18

O) and fix it in position.

on the rear panel, lead it

into a sufficiently large waste bottle and fix it in position.

9 Start up the 833 Pump Unit

• Switch on the 833 Pump Unit with mains switch 8.

• Set the contact pressure for both cassettes: press contact

lever 5 until the solutions are just aspirated. Then press the contact lever up by 1 further click to achieve the optimum contact pressure.

• Check all the tubing from the storage containers to the 833 IC

Liquid Handling Unit and the suppressor module through to the waste bottles for leaks. If any liquid should be leaking then the corresponding connection must be tightened up or replaced.

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

5.1 Connection of the Suppressor module

5 833 IC Liquid

Handling Suppressor Unit

This instrument version can be used for retrofitting a 2.820.0X20 IC Separation Center with two injectors or a 2.761.0010 Compact IC for

chemical suppression in an easy way. It consists of the 833 IC Liquid Handling Unit basic instrument and the 1.753.0100 Metrohm

Suppressor Module MSM.

Suppressor module

Suppressor connection

with permanently attached inlet and outlet capillaries

26 25 24

Fig. 9: Suppressor module 1.753.0100

Connection cable

connection cable to 833 IC Liquid Handling Unit

5.1 Connection of the Suppressor module

The 1.753.0100 Suppressor module must first be inserted in the

2.820.0X20 IC Separation Center and connected to the 833 IC Liquid Handling Unit. Connections are then made to the inlet and outlet capillaries mounted on the suppressor. Proceed as follows (underlined numbers ## Use):

1 Insert suppressor module

refer to parts and controls in the 819/820 Instructions for

• 820.0X20 IC Separation Center (2-channel system):

Place suppressor module 24 inside the chamber on the floor, see Fig. 24, 819/820 Instructions for Use).

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

5 833 IC Liquid Handling Suppressor Unit

2 Connect suppressor module

• 820.0X20 IC Separation Center (2-channel system):

Remove plastic stopper from rear panel opening 18

of the 820 IC Separation Center and lead cable 26 of suppressor module 24 out through one of the openings in the rear panel of the IC Separation Center.

• Connect cable 26 to connection 13 (“Module” of the 833 IC

Liquid Handling Unit (see Fig. 2).

3 Connect the column to the injector

• Remove end caps from column 53

• without column heating:

Screw inlet end of separating column 53 to column connection capillary 50

(note flow direction)

mounted on the injector.

• with column heating:

Prepare column heating according to Section 2.9.2 of the 819/820 Instructions for Use and screw column connection

capillary 50 compression fitting to injection valve 51

(see Fig. 20, 819/820 Instructions for Use) with a

• With precolumn:

Install precolumn according to the supplied leaflet between inlet of the separating column and the injection valve.

H2SO4

Waste

4 Rinse column

• Place a beaker beneath the column outlet.

• Start 818 IC Pumpe 818 in «IC Net» with suitable flow (see

leaflet of the column) and rinse column for ca. 10 min with eluent.

• Stop 818 IC Pump.

Eluent

Waste

Detector

H2O

Suppressor inlet capillary for

eluent

Suppressor inlet capillary for

Suppressor outlet capillary for

Suppressor inlet capillary for

Suppressor outlet capillary for

2SO4

eluent

Fig. 10: Suppressor module connections for 833 IC Liquid Handling

Suppressor Unit

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

5.1 Connection of the Suppressor module

5 Connect column to suppressor module (Suppressor

connection 1)

• Cut inlet capillary 27 (marked with “Eluent”) at suppressor

connection 25 (see Fig. 9) to the required length. Use the

6.2126.080 Capillary cutter available as an option.

• without column heating

Screw inlet capillary 27 on to the outlet end of separating column 53

using a 6.2744.010 compression fitting.

• with column heating

Connect capillary 52

at the outlet of the separating column

(see Fig. 20, 819/820 Instructions for Use) to the inlet capillary 27 using the 6.2744.040 Coupling supplied with the 820 standard equipment.

6 Fix column

• without column heating

Insert one or two column holders 59 or 6.2027.050) in the mounting rails 58

(6.2027.030, 6.2027.040

and fasten separating

column in the column holder.

• with column heating

Insert column heating according to Fig. 10 (819/820 Instructions for Use) into the Separation Center.

7 Connect suppressor module to detector block

(Suppressor connection 1)

• Cut outlet capillary 32 (marked with “Detector”) at suppressor

connection 25 (see Fig. 9) to coupling 71

(6.2620.060) to the required length. Use the 6.2126.080 Capillary cutter available as an option.

• Screw outlet capillary 32 on to coupling 71

by using a

6.2744.010 compression fitting.

• Screw inlet capillary 56

end of coupling 71

of detector block 57 on to the other

8 Attach pump tubing to 833 Liquid Handling Unit

• Mount both the 6.1826.050 Pump tubing (white-yellow

stopper) as described in Section 3.2, see Fig. 7.

9 Suppressor connection 2: H2SO4

• Pull inlet capillary 28 (marked with “H2SO4”) at suppressor

connection 25 (see Fig. 9) through one of the openings 18 the rear panel of the 820 IC Separation Center.

• Attach inlet capillary 28 (23 in Fig. 7) to the filter unit PEEK 22

(6.2821.120) of the first pump tubing using a compression fitting 17 (6.2744.010), see Fig. 7.

• Mount aspiration tubing: cut a piece of PTFE tubing 16

(6.1803.020) to the required length.

• Attach a PEEK compression fitting 17 (6.2744.010) to one

end of the PTFE tubing 16 and screw this on to coupling 18.

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

5 833 IC Liquid Handling Suppressor Unit

• Immerse the other end of the aspiration tubing in a container

with regeneration solution (normally 50 mmol/L H

2SO4

) and fix

it in position.

• Pull outlet capillary 29 (marked with “Waste”) through one of

the openings 41

or 43 in the rear panel of the 820 IC

Separation Center.

• Lead outlet capillary 29 into a sufficiently large waste bottle

and fix it in position.

10 Suppressor connection 3: H2O

• Pull inlet capillary 31 (marked with “H2O”) at suppressor

connection 25 (see Fig. 9) through one of the openings 18

the rear panel of the 820 IC Separation Center.

• Fasten inlet capillary 31 (23 in Fig. 7) to filter unit PEEK 22

(6.2821.120) of the second pump tubing using a compression fitting 17 (6.2744.010), see Fig. 7.

• Mount aspiration tubing: cut a piece of PTFE tubing 16

(6.1803.020) to the required length.

• Attach a PEEK compression fitting 17 (6.2744.010) to one

end of the PTFE tubing 16 and screw this on to coupling 18.

• Immerse the other end of the aspiration tubing in a container

with rinsing solution (normally dist. H

O) and fix it in position.

• Pull outlet capillary 30 (marked with “Waste”) through one of

the openings 41

or 43 in the rear panel of the 820 IC

Separation Center.

• Lead outlet capillary 30 into a sufficiently large waste bottle

and fix it in position.

11 Start up 833 IC Liquid Handling Suppressor Unit

• Switch on 833 Pump Unit with mains switch 8.

• Set the contact pressure for both cassettes: press contact

lever 5 until the solutions are just aspirated. Then press the contact lever up by 1 further click to achieve the optimum contact pressure.

• Before switching the suppressor to the next position for the

first time (see Section 5.2) rinse the three suppressor units with solution for 5 minutes.

• Check all the tubing from the storage containers to the 833 IC

Liquid Handling Unit and the suppressor module through to the waste bottles for leaks. If any liquid should be leaking then the corresponding connection must be tightened up or replaced.

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

5.2 Handling the suppressor module

General

The Metrohm Suppressor Module MSM of the 833 IC Liquid Handling Suppressor Unit consists of a total of three suppressor

units, which are used in sequence for suppression, regenerated with sulfuric acid and rinsed with water. In order to be able to record each chromatogram under comparable conditions, work is normally carried out with a freshly regenerated suppressor. Switching takes place either automatically together with the valve switching or manually.

Correct connection

The three suppressor inlets and outlets numbered 1…3 each have two permanently attached PTFE capillaries that must be connected as described in Section 5.1 (see Fig. 10).

Flow direction

The suppressor units must never be regenerated with H same direction as which the eluent is transported. This is why the inlet and outlet capillaries must always be mounted as described in Section 5.1 and shown in Fig. 10.

Never switch to the next position when dry

The suppressor module must never be switched to the next position when it is dry, as there is a risk that it could be blocked.

No recycling

The recycling method (return of the eluent to the storage container) must not be used with the suppressor.

2SO4

in the

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

6 833 IC Liquid Handling Sample Preparation Unit

6 833 IC Liquid

Handling Sample Preparation Unit

This instrument version consists of the 833 IC Liquid Handling Unit basic instrument and the 1.793.0110 Sample Preparation Module.

Sample preparation module

Sample preparation

connection

with permanently attached inlet and outlet capillaries

Connection cable

3534 33

Fig. 11: 1.793.0110 Sample Preparation Module

connection cable to 833 IC Liquid Handling Unit

6.1 Connection to modular IC system for neutralization

The 833 IC Liquid Handling Sample Preparation Unit is frequently used for the neutralization of an alkaline sample for anion determination with chemical suppression. Excessive amounts of strong bases (e.g. 30% NaOH) should not be fed into the sample preparation module. In order to ensure an adequate capacity for the exchange of Na ions under all circumstances only a small fraction of the sample is fed into the sample preparation module through a sample loop (e.g. 20 µL). The analyte anions are retained on a downstream enrichment column, then re-eluted with the eluent in counterflow and transferred to the separating column.

This means that the necessary instrument configuration corresponds to the Modular IC System 6 (MIC 6 Advanced: anion system with chemical suppression, enrichment and matrix elimination), extended by the 833 IC Liquid Handling Sample Preparation Unit. Samples with a low load for the capacity of the sample preparation module can also be added directly to the sample preparation module and transferred to the sample loop. Switching then corresponds to the system described in Section 6.2.

ions for H+

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

6.1 Connection to modular IC system for neutralization

The electrical connections of this system to the 766 IC Sample Processor with complete control by the «IC Net 2.3» software is described below.

6.1.1 Electrical connections

The electrical connections of the system, consisting of 819 IC Detector, 820 IC Separation Center (2-channel; 2.820.0X20), 818 IC Pump, 833 IC Liquid Handling Pump Unit (2.833.0010), 833 IC Liquid Handling Suppressor Unit (2.833.0020), 833 IC Liquid Handling Sample Preparation Unit (2.833.0030) and 830 IC Interface are shown in Fig. 12:

6.2125.120

6.2143.210

6.2143.200

819

6.2125.090

820

B (LOOP) A (PCC)

6.2128.180

818

6.2141.110

830

6.2134.130

6.2134.040

6.2128.180

6.2134.100

833 Sample Prep

833 Suppressor

6.2115.070

833 Pump

6.2128.180

6.2134.090

Fig. 12: Electrical connections for 833 IC Liquid Handling Sample

Preparation Unit and modular IC system for neutralization

766

6.2134.080

Please note that the signal for switching the connected 833 IC Liquid Handling Suppressor Unit to the next position is not controlled by the program of the 766 Sample Changer. Instead the remote connection 14 of the 833 IC Liquid Handling Suppressor Unit for the Suppressor/Actuator is connected by 6.2128.180 cable with the event line “Fill” of valve B (sample loop before the sample preparation module) to the 820. In this way a move to the next position of the suppressor is triggered by the “Fill” setting of this valve.

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

6 833 IC Liquid Handling Sample Preparation Unit

6.1.2 Connection of the sample preparation module

The following description assumes the use of a 2.820.0X20 IC Separation Center (2-channel system).

The 1.793.0110 Sample Preparation Module must first be inserted in the 820 IC Separation Center and then connected to the basic instrument of the 833 IC Liquid Handling Sample Preparation Unit (833 Sample Preparation in Fig. 12). The 1.753.0100 Suppressor Module of the IC Liquid Handling Suppressor Unit is also inserted in the Separation Center and connected to the relevant basic instrument (833 Suppressor in Fig. 12). This is described in detail in Section 5.

The components are connected as shown below; this also shows the sample flow scheme:

Fill Inject

) Sample loop at valve B

is filled.

B) Sample is neutralized

in Sample Preparation Module; anions are enriched at valve A.

C) Enriched anions are

transferred to the separation column.

Sample

Module

833

Pump

H2O Regenerant RegenerantEluentH2OH

833

Enrichmentcolumn

Inject Fill

Module

833

Pump

O Regenerant RegenerantEluentH2OH

833

Enrichmentcolumn

Inject Inject

Module

Column

818

Column

818

Column

MSM

833

Suppr.

MSM

833

Suppr.

MSM

chment-

833

Pump

O Regenerant RegenerantEluentH2OH

833

column

818

833

Suppr.

The inlet and outlet capillaries mounted on the sample preparation module are connected up as follows:

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

6.1 Connection to modular IC system for neutralization

1 Insert sample preparation module

• Place sample preparation module 33 inside the chamber on

the floor.

2 Connect sample preparation module

• Remove plastic stoppers from the rear panel openings 18 of

the 820 IC Separation Center and lead cable 35 mounted on sample preparation module 33 back through this opening.

• Connect cable 35 to connection 13 “Module” of the 833 IC

Liquid Handling Unit (see Fig. 2).

3 Connect sample feed to sample preparation

module (Sample Preparation connection 1)

• Connect inlet capillary 36 (marked with “Sample in”) at the

sample preparation module connection 34 (see Fig. 13) to connection “5” of injection valve B using a 6.2744.010 compression fitting.

4 Connect sample preparation module to valve A

(enrichment column) (Sample Preparation connection 1)

• Connect outlet capillary (marked “Sample out”) at sample

preparation module connection 34 (see Fig. 13) to connection “1” of injection valve A using a 6.2744.010 compression fitting.

• When making the further connections to injection valve A

make sure that the ”Inject” setting of the enrichment column is rinsed in the reverse direction to the “Fill” setting.

Regenerant

Waste

Sample in

Inlet capillary for sample

Inlet capillary for acid

Outlet capillary for acid

Outlet capillary for H

Inlet capillary for H

Sample out

H2O

Outlet capillary for sample

Waste

Fig. 13: Connections at sample preparation module of the 833 IC Liquid

Handling Sample Preparation Unit

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

6 833 IC Liquid Handling Sample Preparation Unit

5 Mount pump tubing on the 833 Liquid Handling Unit

• Mount the two lengths of 6.1826.010 Pump tubing (white-

white stopper) as described in Section 3.2, see Fig. 7.

6 Sample preparation module connection 2:

Regenerant

• Pull inlet capillary 37 (marked with “Regenerant”) at sample

preparation module connection 34 (see Fig. 13) through one of the openings 18

on the rear panel of the 820 IC Separation

Center.

• Attach inlet capillary 37 (23 in Fig. 7) to filter unit PEEK 22

(6.2821.120) of the first pump tubing using a compression fitting 17 (6.2744.010), see Fig. 7.

• Mount aspiration tubing: cut a piece of PTFE tubing 16

(6.1803.020) to the required length.

• Attach a PEEK compression fitting 17 (6.2744.010) to one

end of the PTFE tubing 16 and screw this on to coupling 18, see Fig. 7.

• Immerse the other end of the aspiration tubing in a container

with regeneration solution (normally 20 mmol/L perchloric acid) and fix it in position.

• Pull outlet capillary 38 (marked with “Waste”) at sample

preparation module though one of the openings 18

of the

rear panel of the 820 IC Separation Center.

• Lead outlet capillary 38 into a sufficiently large waste bottle

and fix it in position.

7 Sample preparation module connection 3: H2O

• Pull inlet capillary 40 (marked with “H2O”) at Sample

preparation module connection 34 (see Fig. 13) through one of the openings 18

on the rear panel of the 820 IC Separation

Center.

• Attach inlet capillary 40 (23 in Fig. 7) to the filter unit PEEK 22

(6.2821.120) of the second pump tubing using a PEEK compression fitting 17 (6.2744.010), see Fig. 7.

• Mount aspiration tubing: cut a piece of PTFE tubing 16

(6.1803.020) to the required length.

• Attach a PEEK compression fitting 17 (6.2744.010) to one

end of the PTFE tubing 16 and screw this on to coupling 18, see Fig. 7.

• Immerse the other end of the aspiration tubing in a container

with rinsing solution (normally deionized water) and fix it position.

• Pull outlet capillary 39 (marked with “Waste”) at Sample

preparation module connection 34 (see Fig. 13) through one of the openings 18

in the rear panel of the 820 IC Separation

Center.

• Lead outlet capillary 39 into a sufficiently large waste bottle

and fix it in position.

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

6.1 Connection to modular IC system for neutralization

8 Start-up 833 IC Liquid Handling Sample Preparation

Unit

• Switch on 833 LH Pump Unit with mains switch 8.

• Set the contact pressure for both cassettes: press contact

lever 5 until the solutions are just aspirated. Then press the contact lever up by 1 further click to achieve the optimum contact pressure.

• Check all the tubing from the storage containers to the 833 IC

Liquid Handling Unit and the sample preparation module through to the waste bottles for leaks. If any liquid should be leaking then the corresponding connection must be tightened up or replaced.

• Before the sample preparation module is used for the first

time the cation exchanger material must be conditioned. This is done by injecting e.g. 30% NaOH 15 times (5 injections per unit). You can use the program described in the following section for the system “Neutralisation.smt” with a running time of 20 min; the column does not need to be mounted.

6.1.2.2 Settings in IC Net

When setting up the 833 IC Liquid Handling Sample Preparation Unit and the 833 IC Liquid Handling Unit the “New system wizard” of the IC Net program demands the assignment of an “Event line” for the sample preparation module and the suppressor module. Although this does not exist you should still select any unused Event line so that the “New system wizard” can continue. In fact the sample preparation module is controlled from the 766 IC Sample Processor and the suppressor module from the Event Line of the 820 valve B (see Fig. 12).

Apart from the main program “Neutralisation.smt” two further programs should be created for the 766 IC Sample Processor in separate system files. The 766 program in the system file “Start-Neutralisation.smt” only starts the peristaltic pump (833 Pump) and rinses the sample preparation module in all three positions. “End-Neutralisation.smt” switches the pump off (833 Pump).

The peristaltic pumps of the 833 IC Liquid Handling Sample Preparation Unit (833 Sample Prep) and the 833 IC Liquid Handling Suppressor Unit (833 Suppressor, see Fig. 12) start immediately when the system is activated (recording the baseline). This is done by activating the option ’Start pump with startup hardware’ in IC Net for each instrument.

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

6 833 IC Liquid Handling Sample Preparation Unit

Neutralisation.smt

1. Program input for the 766 IC Sample Processor:

001 Ctrl INIT 819 002 Move sample 003 Lift work 004 Ctrl FILL B / STEP 1 005 Pump 120 s 006 Ctrl FILL A 1 007 Ctrl INJECT B1 008 Wait 60 s

009 Ctrl ZERO 1 010 Ctrl INJECT A1 011 Ctrl STEP MSM 833

(*) The time for transferring the sample via the sample preparation module must

be adequate, but should be kept as short as possible in order to minimize contamination of the downstream enrichment column with unwanted anions from the water used. This is also the reason why the blank value of this water should be measured regularly for calibration purposes.

Start-Neutralisation.smt

2. Save the system “Neutralisation.smt” under a new name “StartNeutralisation.smt”.

− Initializes remote lines at 819

− Moves needle to sample position

− Moves lift with needle to working position

− Switches injection valve B at 820 to "Fill"

− Transfers sample to first sample loop

− Switches injection valve A at 820 to "Fill"

− Switches injection valve B at 820 to "Inject"

− Transfers sample via sample preparation module to

enrichment column (*)

− Triggers autozero at 819 IC Detector

− Switches injection valve A at 820 to "Inject"

− Switches sample preparation module to next position

3. Remove the data recorder by clicking on the recorder icon with the right-hand mouse key and then selecting “Unlink”.

4. Change the program for 'Start-Neutralisation.smt' as follows and save it again:

001 Ctrl INIT 819 002 Ctrl PUMP 833 on 003 Wait 300 s 004 Ctrl STEP MSM 833 005 Wait 300 s 006 Ctrl STEP MSM 833 007 Wait 300 s

End-Neutralisation.smt

5. Save the system “Start-Neutralisation.smt” under a new name “EndNeutralisation.smt”.

6. Change the program for “End-Neutralisation.smt” as follows and save it again:

001 Ctrl INIT 819 002 Ctrl PUMP 833 off

− Initializes remote lines at 819

− Switches on 833 Pump Unit 833

− Rinsing time

− Switches sample preparation module to next position

− Rinsing time

− Switches sample preparation module to next position

− Rinsing time

− Initializes remote lines at 819

− Switches off 833 Pump Unit 833

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

6.2 Connection to modular IC system for cation separation

7. The sample queue to be processed then contains the following entries, for example:

System Ident Vial Chrom. No.

1 Start-Neutralisation.smt dummy 1 - 2 Neutralisation.smt Sample 1 1 1 3 Neutralisation.smt Sample 2 2 2 4 Neutralisation.smt Sample 3 3 3 5 Neutralisation.smt Sample 4 4 4 6 Neutralisation.smt Sample 5 5 5 7 End-Neutralisation.smt dummy 5 -

This example shows the processing of a sample series with 5 samples. the 'Chrom. No.' column is only used for information.

6.2 Connection to modular IC system for cation separation

A further application for the 833 IC Liquid Handling Sample Preparation Unit is the separation of cations before injecting the sample onto the separation column (e.g. separation of heavy metals). A system for the determination of anions with chemical suppression is described, in which the direct transfer of the sample to the sample preparation module with subsequent transfer of the treated sample to the injection valve is planned. This is why the necessary instrument configuration corresponds to that of the Modular IC System 2 (MIC 2 Advanced: anion system with chemical suppression), extended by the 833 IC Liquid Handling Unit.

If you are not certain whether the capacity of the sample preparation module is sufficient for your application then, for more strongly polluted samples which require matrix elimination and enrichment, you should use such a system as that described in Section 6.1.

The electrical connections of the system described above to the 766 IC Sample Processor with complete control by the «IC Net 2.3» software is described below.

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

6 833 IC Liquid Handling Sample Preparation Unit

6.2.1.1 Electrical connection

The electrical connections of the system, consisting of 819 IC Detector, 820 IC Separation Center (2.820.0X30; 1-channel + MSM), 818 IC Pump, 833 IC Liquid Handling Pump Unit, 833 IC Liquid Handling Sample Preparation Unit and 830 IC Interface are shown in Fig. 14:

6.2125.120

6.2143.210

819

6.2125.090

820

6.2115.070

818

766

6.2141.110

6.2134.080

830

6.2134.130

6.2134.040

6.2128.180

6.2134.100

833 Sample Prep

833 Pump

6.2128.180

6.2134.090

Fig. 14: Connection of 833 IC Liquid Handling Sample Preparation Unit

to modular IC system for cation separation

6.2.1.2 Connection of the sample preparation module

The following description assumes the use of a 2.820.0X30 IC Separation Center (1-channel system, MSM).

The 1.793.0110 Sample Preparation Module must first be inserted in the 820 IC Separation Center and connected to the basic instrument of the 833 IC Liquid Handling Sample Preparation Unit (833 Sample

Preparation in Fig. 14).

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

6.2 Connection to modular IC system for cation separation

The components are connected as shown below; this also shows the sample flow scheme:

Fill

) Cations of the sample

are continuously

exchanged for H

ions in the ssample preparation module; sample loop at valve A is filled.

B) Sample is neutralized

in sample preparation module; anions are enriched at valve A.

The inlet and outlet capillaries mounted on the sample preparation

module are connected as follows:

Sample

Regenerant H

Module

833

Module

833

Column

818

RegenerantEluent H

MSM

833

Pump

ORegenerant H2O

Inject

Column

818

RegenerantEluent H2O

MSM

833

Pump

1 Insert sample preparation module

• Place sample preparation module 33 inside the chamber on

the floor.

2 Connect sample preparation module

• Remove plastic stoppers from the rear panel openings 18 of

the 820 IC Separation Center and lead cable 35 mounted on sample preparation module 33 back through this opening.

• Connect cable 35 to connection 13 “Module” of the 833 IC

Liquid Handling Unit (see Fig. 2).

3 Connect sample feed to sample preparation

module (Sample Preparation connection 1)

• Connect inlet capillary 36 (marked with “Sample in”) at

sample preparation module connection 34 (see Fig. 13) to the 766 Autosampler using the 6.1831.060 PEEK capillary, two 6.2744.010 compression fittings and a 6.2744.040 PEEK coupling.

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

6 833 IC Liquid Handling Sample Preparation Unit

4 Connect sample preparation module to valve A

(Sample Preparation connection 1)

• Connect outlet capillary 41 (marked with “Sample out”) at

sample preparation module connection 34 (see Fig. 13) to connect “1” of injection valve A using a 6.2744.010 compression fitting.

5 Mount pump tubing on 833 Liquid Handling Unit

• Mount the two lengths of 6.1826.010 Pump tubing (white-

white stopper) as described in Section 3.2, see Fig. 7.

6 Sample preparation module connection 2:

Regenerant

• Pull inlet capillary 37 (marked with “Regenerant”)at sample

preparation module connection 34 (see Fig. 13) through one of the openings 18

on the rear panel of the 820 IC Separation

Center.

• Attach inlet capillary 37 (23 in Fig. 7) to filter unit PEEK 22

(6.2821.120) of the first pump tubing using a compression fitting 17 (6.2744.010), see Fig. 7.

• Mount aspiration tubing: cut a piece of PTFE tubing 16

(6.1803.020) to the required length.

• Attach a PEEK compression fitting 17 (6.2744.010) to one

end of the PTFE tubing 16 and screw this on to coupling 18, see Fig. 7.

• Immerse the other end of the aspiration tubing in a container

with regeneration solution (normally 50 mmol/L perchloric acid) and fix it in position.

• Pull outlet capillary 38 (marked with “Waste”) at sample

preparation module though one of the openings 18

of the

rear panel of the 820 IC Separation Center.

• Lead outlet capillary 38 into a sufficiently large waste bottle

and fix it in position.

7 Sample preparation module connection 3: H2O

• Pull inlet capillary 40 (marked with “H2O”) at sample

preparation module connection 34 (see Fig. 13) through one of the openings 18

on the rear panel of the 820 IC Separation

Center.

• Attach inlet capillary 40 (23 in Fig. 7) to the filter unit PEEK 22

(6.2821.120) of the second pump tubing using a PEEK compression fitting 17 (6.2744.010), see Fig. 7.

• Mount aspiration tubing: cut a piece of PTFE tubing 16

(6.1803.020) to the required length.

• Attach a PEEK compression fitting 17 (6.2744.010) to one

end of the PTFE tubing 16 and screw this on to coupling 18, see Fig. 7.

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

6.2 Connection to modular IC system for cation separation

• Immerse the other end of the aspiration tubing in a container

with rinsing solution (normally deionized water) and fix it position.

• Pull outlet capillary 39 (marked with “Waste”) at sample

preparation module connection 34 (see Fig. 13) through one of the openings 18

in the rear panel of the 820 IC Separation

Center.

• Lead outlet capillary 39 into a sufficiently large waste bottle

and fix it in position.

8 Start-up 833 IC Liquid Handling Sample Preparation

Unit

• Switch on 833 LH Pump Unit with mains switch 8.

• Set the contact pressure for both cassettes: press contact

lever 5 until the solutions are just aspirated. Then press the contact lever up by 1 further click to achieve the optimum contact pressure.

• Check all the tubing from the storage containers to the 833 IC

Liquid Handling Unit and the sample preparation module through to the waste bottles for leaks. If any liquid should be leaking then the corresponding connection must be tightened up or replaced.

• Before the sample preparation module is used for the first

6.2.2 Settings in IC Net

When setting up the 833 IC Liquid Handling Sample Preparation Unit

and the 833 IC Liquid Handling Unit the “New system wizard” of the IC

Net program demands the assignment of an “Event line” for the

Actuator, i.e. the sample preparation module. Although this does not

exist you should still select any unused Event line so that the “New

system wizard” can continue. In fact the sample preparation module is

controlled from the 766 IC Sample Processor (see Fig. 14).

The signal for switching the internal suppressor module of the 820 to

the next position is not controlled by the program of the 766 IC Sample

Changer. Instead the parameter “Auto Step” is set to “fill” in the

parameter window of the 820 IC Separation Center in IC Net (double-

click on 820 symbol).

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

6 833 IC Liquid Handling Sample Preparation Unit

The peristaltic pumps of the 833 IC Liquid Handling Pump Unit and the 833 IC Liquid Handling Sample Preparation Unit start immediately when the system is activated (recording the baseline). This is done by activating the option

’Start pump with startup hardware’ in IC Net for each

instrument.

Catex.smt

The program for the 766 IC Sample Processor is as follows:

001 Ctrl INIT 819 002 Move sample 003 Lift work 004 Ctrl ZERO 1 005 Ctrl FILL A 1 006 Pump 120 s

007 Ctrl INJECT A1 008 Ctrl STEP MSM 833

(*) The time for transferring the sample via the sample preparation module must

be adequate, but should be kept as short as possible in order to minimize contamination of the downstream enrichment column with unwanted anions from the water used.

− Initializes remote lines at 819

− Moves needle to sample position

− Moves lift with needle to working height

− Triggers autozero at 819 IC Detector

− Switches injection valve A at 820 to "Fill"

− Transfers sample to sample loop via sample

preparation module (*)

− Switches injection valve A at 820 to "Inject"

− Switches sample preparation module to next

position

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

6.3 Handling the sample preparation module

General

The sample preparation module of the 833 IC Liquid Handling

Sample Preparation Unit contains a total of three cartridges, which

are used in sequence for exchanging cations, for regeneration, and for

rinsing with water. In order to be able to record each chromatogram

under comparable conditions work is normally carried out with a freshly

regenerated cartridge. Switching takes place either automatically

together with the valve switching or manually.

Correct connection

The three actuator unit inlets and outlets numbered 1, 2, 3 each have

two permanently attached PTFE capillaries that must be connected as

described in Section 6.1 and 6.2 (see Fig. 13).

Flow direction

The cation exchanger units of the sample preparation module must never be regenerated in the same flow direction as that in which the sample is transported. This is why the inlet and outlet capillaries must always be mounted as described in Section 6.1 and 6.2 and shown in Fig. 13.

Never switch to the next position when dry

The sample preparation module must never be switched to the next position when it is dry, as there is a risk that it could be blocked.

No recycling

The recycling method (return of the eluent to the storage container) must not be used with the sample preparation module.

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

7 833 IC Liquid Handling Dialysis Unit

7 833 IC Liquid

Handling Dialysis Unit

This version consists of the 833 IC Liquid Handling Unit basic instrument and the 6.2729.100 Dialysis Cell.

47 46 45 44 43 42

50 49 48 48 52 51

Fig. 15: 6.2729.100 Dialysis Cell

6.2729.100 Dialysis cell

Upper part of dialysis cell

E.301.0111 Sealing ring

6.2714.010 Dialysis membrane

Lower part of dialysis cell

V.022.6030 Screw with 4.754.4090

Washer

A dialysis system with manual sample injection is described below.

Slot for holding the dialysis cell in

cell holder 6

Outlet for acceptor solution

Inlet for acceptor solution

Inlet for sample solution

Outlet for sample solution

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

7.1 Flow diagram for dialysis

Sample dialysis with the 833 IC Liquid Handling Dialysis Unit comprises

the following four steps for each sample:

1 Rinsing

Valve A: INJECT

Waste

Sample channel, acceptor channel and

Inject

sample loop are rinsed (for approx. 2 min).

Colum

Eluent

2 Dialysis with «stopped flow»

Valve A: INJECT

Waste

The sample is dialyzed with stationary acceptor

Inject

solution (dialysis time approx. 10 min).

Colum

Eluent

833

Dialysis

Unit

833

Dialysis

Unit

cceptor

Sample

833

Pump

Unit

833

Pump

Unit

Waste

3 Transfer to sample loop

Valve A: FILL

The acceptor solution enriched with ions from

Fill

the sample is transferred to the sample loop (transfer time approx. 0.5 min).

Colum

Eluent

4 Injection

Valve A: INJECT

The acceptor solution

Inject

enriched with ions from the sample is injected into the IC system.

Colum

Eluent

Waste

Dialysis

Unit

833

Dialysis

Unit

833

cceptor

Sample

833

Pump

Unit

833

Pump

Unit

Waste

To perform dialysis with the 833 IC Liquid Handling Dialysis Unit two

peristaltic pumps are required. One pump (833 Dialysis Unit) is

delivering the acceptor solution, the other one (833 Pump Unit) is

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

7 833 IC Liquid Handling Dialysis Unit

delivering the sample. One channel of each pump is used to transfer solution to the dialysis cell, the second channel is required to remove solution from the dialysis cell. This setup ensures constant flow and equal pressure conditions on both sides of the dialysis membrane.

7.2 Electrical connection

7.2.1 Dialysis without suppression

The electrical connections of the system, consisting of 819 IC Detector, 820 IC Separation Center (2.820.0X10; 1-channel), 818 IC Pump, 833 IC Liquid Handling Dialysis Unit, 833 IC Liquid Handling Pump Unit and 830 IC Interface are shown in Fig. 16:

819

820

6.2125.090

6.2115.070

818

830

6.2134.130

6.2143.210

6.2134.040

833 Pump

6.2134.100

833 Dialysis

6.2134.090

Fig. 16: Connecting the 833 IC Liquid Handling Dialysis Unit to a modular

dialysis system without suppression

Make sure that the remote control of the peristaltic pumps 833 Pump and 833 Dialysis via 6.2143.210 cable (see Section 3.1.2) corresponds to the remote configuration of the detector program (see Section 7.3.1).

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

7.2 Electrical connection

7.2.2 Dialysis with suppression

The electrical connections of the system, consisting of 819 IC Detector,

820 IC Separation Center (2.820.0X30; 1-channel with suppressor), 818

IC Pump, 833 IC Liquid Handling Suppressor Unit (2 x), 833 IC Liquid

Handling Dialysis Unit and 830 IC Interface is shown in Fig. 17:

819

820

6.2125.090

6.2115.070

818

830

6.2134.130

6.2134.040

6.2128.180

6.2134.100

6.2134.090

6.2143.210

833 Pump

833 Dialysis

(Suppressor)

Fig. 17: Connecting the 833 IC Liquid Handling Dialysis Unit to a modular

dialysis system with suppression

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

7 833 IC Liquid Handling Dialysis Unit

7.3 Settings in IC Net

7.3.1 Dialysis without suppression

The program steps required for dialysis are all controlled by the time program of the 819 IC Detector.

Start of 833 Pump (Sample)

Rinse time

Dialysis time

Transfer time

Start of 833 Pump (Acceptor)

Stop of acceptor solution

Trigger auto-zero at 819 Detector

Fill sample loop

Transfer to sample loop

Injection (Start evaluation)

Stop of 833 Pump (Acceptor)

Stop of 833 Pump (Sample)

Fig. 18: Time program for dialysis without suppression

Make sure that the remote control of the peristaltic pumps 833 Pump and 833 Dialysis (see Section 7.2.1) via the 6.2143.210 cable (see Section 3.1.2) corresponds to the remote configuration of the detector program.

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

7.3 Settings in IC Net

7.3.2 Dialysis with suppression

The peristaltic pump of the 833 IC Liquid Handling Suppressor Unit

(833 Suppressor see Fig. 17) starts immediately when the system is

activated (recording the baseline). This is done by activating the option

’Start pump with startup hardware’ for the instrument in IC Net.

The program steps required for dialysis are all controlled by the time

program of the 819 IC Detector.

Start of 833 Pump (Sample)

Rinse time

Dialysis time

Transfer time

Start of 833 Pump (Acceptor)

Stop of acceptor solution

Switch suppressor to next position

Trigger auto-zero at 819 Detector

Fill sample loop

Transfer to sample loop

Injection (Start evaluation)

Stop of 833 Pump (Acceptor)

Stop of 833 Pump (Sample)

Fig. 19: Time program for dialysis with suppression

Make sure that the remote control of the peristaltic pumps 833 Pump and 833 Dialysis (see Section 7.2.2) via the 6.2143.210 cable (see Section 3.1.2) corresponds to the remote configuration of the detector program.

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

7 833 IC Liquid Handling Dialysis Unit

7.4 Assembling the dialysis cell

This section describes the initial assembly of the dialysis cell. Before it is used a dialysis membrane must be inserted. This is done as follows (see Fig. 15):

1 Prepare dialysis cell

• Remove dialysis cell 42 (6.2729.100) from the packaging and

screw out the four 6.2744.060 Blank stoppers .

• Use the 6.2621.070 Allen key to loosen the 5 screws 47

completely, remove lower part 46 from upper part 43 and remove sealing ring 44.

2 Clean dialysis cell

• Thoroughly rinse sealing ring 44, upper part 43 and lower

part 46 of the dialysis cell with ultrapure water and dry with N or a lint-free tissue.

Only ultrapure water or ethanol should be used for cleaning the dialysis cell, other organic solvents (e.g. acetone) will damage the Plexiglas cell!

3 Prepare dialysis membrane

• Use the 6.2831.010 Tweezers to remove a new dialysis

membrane 45 (e.g. 6.2714.010) from the packaging and immerse in a Petri dish filled with ultrapure water for approx. 2 min until the membrane is thoroughly soaked with water.

4 Insert dialysis membrane

• Place upper part 43 on a paper tissue with its inner side

uppermost.

• Place sealing ring 44 in the recess provided for it in upper

part 43.

• Use the 6.2831.010 Tweezers to place the wet dialysis

membrane 45 (e.g. 6.2714.010) inside sealing ring 44 on upper part 43.

Make sure that the dialysis membrane soaked with water does not dry out before insertion as otherwise it cannot be used !

5 Close dialysis cell

• Place lower part 46 on upper part 43 so that the two parts are

properly aligned with each other.

• Use the 6.2621.070 Allen key to screw in the 5 screws 47

completely and tighten them up well.

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

7.5 Making the capillary connections

6 Assemble dialysis cell

• Push the 6.2057.010 Cell holder into the free folding guide of

the 820 IC Separation Center and insert assembled dialysis cell 42 in the holder.

Fig. 20 Inserting the dialysis cell in the holder

7.5 Making the capillary connections

7.5.1 Preparing the 820 IC Separation Center

For operation with the 833 IC Liquid Handling Dialysis Unit the 820 IC

Separation Center must be converted as follows (see Fig. 21):

1 Dismantle accessories

• Pull the PTFE aspiration tube completely out of the

feedthrough 14

56.

• Dismantle the PEEK capillary tubing from connection "2" of

valve A 56 to the feedthrough 13

2 Make connections to suppressor (only for

2.820.0X30)

• Install suppressor module of the 820 IC Separation Center

and the additional 833 IC Liquid Handling Pump Unit as described in Section 4.

and screw it off from connection "1" of valve A

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

7 833 IC Liquid Handling Dialysis Unit

7.5.2 Connection of the dialysis cell

820

Column

Eluent

833 Dialysis

833 Pump

Acceptor

Sample

Fig. 21: Tubing connection system

6.1803.040 PTFE capillary (1 m)

for supplying sample/acceptor solution

6.2744.010 PEEK compression

fitting

18 6.2744.034 Coupling

6.2744.160 PEEK coupling with

tubing security device

42 6.2729.100 Dialysis cell

6.1826.030 Pump tubing

(19 in Fig. 7) with orange-yellow stoppers for transferring the acceptor solution

6.1826.040 Pump tubing

(19 in Fig. 7) with black-black stoppers for transferring the sample

6.1825.210 PEEK sample loop

(20 µL )

Injection valve A

6.1803.040 PTFE capillary (1 m)

connection peristaltic pump (channel 1 of 833 Pump Unit for the supply of

fresh sample) – inlet dialysis cell (sample side)

Waste

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

7.5 Making the capillary connections

6.1803.040 PTFE capillary (1 m)

connection outlet dialysis cell (sample side) – peristaltic pump (channel 2 of 833 Pump Unit for the disposal of dialyzed sample solution)

PTFE capillary 6.1803.040 (1 m)

connection peristaltic pump (channel 2 of 833 Pump Unit for the disposal

of dialyzed sample solution) – waste container

6.1803.040 PTFE capillary (1 m)

connection peristaltic pump (channel 1 of 833 Dialysis Unit for the supply

of fresh acceptor solution) – inlet dialysis cell (acceptor side)

To connect dialysis cell 42 to the IC system proceed as follows (see

also Fig. 21):

6.1831.050 PEEK capillary (40 cm)

connection outlet dialysis cell (acceptor side) – connection “1” of valve A

6.1831.060 PEEK capillary (1 m)

connection of connection “2” valve A – peristaltic pump (channel 2 of 833 Dialysis Unit for the disposal of acceptor solution)

6.1803.040 PTFE capillary (1 m)

peristaltic pump (channel 2 of 833 Dialysis Unit for the disposal of acceptor solution) – waste container

6.2744.000 PVDF compression fitting

Waste container

Capillaries fitted with new connectors must have a perfectly flat cut surface. Use the 6.2621.080 Capillary cutter available as an option to cut capillaries.

Connections for sample solution

1 Attach pump tubing to 833 Liquid Handling Pump

Unit

• Attach the two pieces of pump tubing 6.1826.040 (black-

black stopper) as described in Section 3.2 to the 833 IC Liquid Handling Pump Unit 833, see Fig. 7.

2 Connect aspiration capillary for sample

• Attach one end of aspiration capillary 16 (6.1803.040; L =1

m) to PEEK coupling 18 on the suction side of the black- black pump tubing of channel 1 from the 833 Pump Unit using a PEEK compression fitting 17 (6.2744.010) (see Fig. 7 and Fig. 21).

• Immerse the other end of aspiration tubing 16 in the sample

container and fix it in position.

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

7 833 IC Liquid Handling Dialysis Unit

3 Connect dialysis cell

• Screw PTFE capillary 57 (6.1803.040; L =1 m) (23 in Fig. 7)

to PEEK coupling 21 (6.2744.034) on the delivery side of the pump tubing with the black-black stoppers of channel 1 from the 833 Pump Unit using a PEEK compression fitting 17 (6.2744.010) (see Fig. 7 and Fig. 21). Lead the other end of the capillary through one of the feedthroughs 14

at the front or the side of the 820 Separation Center in the column compartment and screw it on to inlet opening 51 of lower part 46 of the dialysis cell using a PVDF compression fitting 64 (6.2744.000) (see Fig. 15 and Fig. 21).

• Screw PTFE capillary 58 (6.1803.040; L =1 m) to outlet

opening 52 of lower part 46 of the dialysis cell (see Fig. 15) using a PVDF compression fitting 64 (6.2744.000) and lead it out of the column compartment through one of the feedthroughs 14

on the front or side of the 820 Separation Center. Attach the other end of the PTFE capillary 58 to PEEK coupling 18 on the suction side of the black-black pump tubing of channel 2 from the 833 Pump Unit using a PEEK compression fitting 17 (6.2744.010) (see Fig. 7 and Fig. 21).

Use only the above-mentioned 6.2744.000 PVDF compression fittings for the dialysis cell connections. If 6.2744.010 PEEK

compression fittings are used then stress cracks could occur in the dialysis cell !

4 Connect waste container

• Screw PTFE capillary 59 (6.1803.040; L =1 m) (23 in Fig. 7)

to PEEK coupling 21 (6.2744.034) on the delivery side of the pump tubing with the black-black stoppers of channel 2 from the 833 Pump Unit using a PEEK compression fitting 17 (6.2744.010) (see Fig. 7 and Fig. 21). Lead the other end of the capillary into a sufficiently large waste container and fix it in position.

Connections for acceptor solution

1 Connect pump tubing to 833 Liquid Handling

Dialysis Unit

• Attach the two pieces of pump tubing 6.1826.030 (orange-

yellwo stopper) as described in Section 3.2 to the 833 IC Liquid Handling Dialysis Unit 833, see Fig. 7.

2 Connect aspiration capillary for acceptor solution

• Attach one end of aspiration capillary 16 (6.1803.040; L =1

m) to PEEK coupling 18 on the suction side of the orange-

yellow pump tubing of channel 1 from the 833 Dialysis Unit using a PEEK compression fitting 17 (6.2744.010) (see

Fig. 7 and Fig. 21).

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

7.5 Making the capillary connections

• Immerse the other end of aspiration tubing 16 in the sample

container and fix it in position. Ultrapure water is normally

used as the acceptor solution; it must first be degassed (with N

, He or vacuum).

3 Connect dialysis cell

• Screw PTFE capillary 60) (6.1803.040; L =1 m) to PEEK

coupling 21 (6.2744.034) on the delivery side of the pump tubing with the orange-yellow stoppers of channel 1 from the 833 Dialysis Unit using a PEEK compression fitting 17 (6.2744.010) (see Fig. 7 and Fig. 21). Lead the other end of the capillary through one of the feedthroughs 14

at the front or the side of the 820 Separation Center in the column compartment and screw it on to inlet opening 50 of upper part 43 of the dialysis cell with a PVDF compression fitting 64 (6.2744.000) (see Fig. 15 and Fig. 21).

• Screw PEEK capillary 61 (6.1831.050; L =40 cm)(see Fig. 21)

to outlet opening 49 of cell upper part 43 of the dialysis cell using a PVDF compression fitting 64 (6.2744.000) (see Fig.

15).

Use only the above-mentioned 6.2744.000 PVDF compression fittings for the dialysis cell connections. If 6.2744.010 PEEK compression fittings are used then stress cracks could occur in the dialysis cell !

4 Connect injection valve

• Screw the PEEK capillary 61 (6.1831.050; L = 40 cm)

attached to outlet 49 to connection "1" of valve A 56 using a

6.2744.010 PEEK compression fitting.

• Screw PEEK capillary 62 (6.1831.060; L =1 m) to connection

"2" of valve A 56 using a 6.2744.010 PEEK compression fitting and lead it out of the column compartment through one of the feedthroughs 14

on the front or side of the 820

Separation Center. Attach the other end of the PTFE capillary

62 to PEEK coupling 18 on the suction side of the orange- yellow pump tubing of channel 2 from the 833 Dialsis Unit

using a PEEK compression fitting 17 (6.2744.010) (see Fig. 7 and Fig. 21).

5 Connect waste container

• Screw PTFE capillary 63 (6.1803.040; L =1 m) (23 in Fig. 7)

to PEEK coupling 21 (6.2744.034) on the delivery side of the pump tubing with the orange-yellow stoppers of channel 2 from the 833 Dialysis Unit using a PEEK compression fitting 17 (6.2744.010) (see Fig. 7 and Fig. 21). Lead the other end of the capillary into a sufficiently large waste container and fix it in position.

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

7 833 IC Liquid Handling Dialysis Unit

Conditioning the dialysis system

Before the first analysis the dialysis cell with the inserted dialysis membrane and all the tubing connections must be rinsed with ultrapure water. Proceed as follows:

1 Settings at 820 IC Separation Center

• Switch injection valves A and B in the 820 IC Separation

Center to the setting "FILL" in the «IC Net» software.

2 Start-up the 833 IC Liquid Handling Dialysis Unit

• Immerse the 2 pieces of aspiration tubing 16 (see Fig. 21) in

the acceptor solution (degassed ultrapure water).

• Switch on 833 Liquid Handling Pump Unit and 833 IC Liquid

Handling dialysis Unit with mains switch 8.

• Start the peristaltic pumps in «IC Net» by setting the remote

line 1 (833 Pump Unit) and remote line 2 (833 Dialysis Unit) in the window of the 819 Detector.

• Set the contact pressure for both cassettes: press contact

lever 5 until the solutions are just aspirated. Then press the contact lever up by 1 further click to achieve the optimum contact pressure.

• Rinse the dialysis system for approx. 10 min with ultrapure

water and check that the same amount of solution emerges from both the waste outlets in the waste bottle.

3 Conditioning the dialysis membrane

• Rinse the dialysis system for approx. 20 min with ultrapure

water. Check that the same amount of solution emerges from both the waste outlets in the waste bottle.

• Check all tubing from the storage containers to the tubing

cassettes and dialysis cell and up to the waste bottle for leaks. If any leaks are found then the corresponding connection must either be tightened up or replaced.

• If any air bubbles remain in the dialysis cell then screw off

PEEK tubing 62 (acceptor solution) and PTFE tubing 58 (sample) from outlets 49 and 52 of the dialysis cell and wait until the air bubbles have vanished. Then screw the tubing back on again.

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

7.6 Optimizing the dialysis

7.6.1 Determining the rinsing time

A rinsing time of 2 min is normally sufficient for completely rinsing the sample and acceptor channels. This time can be increased if necessary.

7.6.2 Determining the transfer time

The time for transferring the enriched acceptor solution to the sample loop must be chosen so that the part of the acceptor solution with the highest ion concentration is transferred to the sample loop. The following values can normally be used for the optimal transfer time if the standard accessories are used; they depend on the delivery rate of the pump:

Mains frequency Optimal transfer time

50 Hz 0.5 min 60 Hz 0.4 min

You should determine the optimal transfer time yourself for each analytical problem by measuring the individual ion concentrations as a function of the transfer time and checking them from time to time. Proceed as follows:

1 First measurement

• Set transfer time in program to 0.2 min and dialysis time to 10

min (see Section 7.3.1/7.3.2).

• Immerse sample

standard containing 10 mg/L of the particular anion or cation.

• Start determination in IC Net and wait until chromatogram has

been evaluated.

2 Further measurements

• Increase the transfer time in the program (see

Section 7.3.1/7.3.2) in steps of 0.1 min until the measured concentration starts to decrease.

• Carry out measurements as described in item 1.

3 Determine the optimal transfer time

• Plot the measured peak area or concentration as a function

of the transfer and determine the optimal transfer time from the plot.

aspiration tubing 16 (see Fig. 21) in a

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

7 833 IC Liquid Handling Dialysis Unit

The below illustration shows an example of such a determination for anions using the 6.2714.010 Dialysis membrane from Metrohm (cellulose acetate; thickness= 115 µm; pore size= 0.2 µm). A standard solution containing 10 mg/L of each of the individual anions was used as the sample and dialyzed for10 min (mains frequency 50 Hz).

12.0

10.0

8.0

6.0

4.0

Konzentration [mg/L]

2.0

0.0

0.00.10.20.30.40.50.60.70.80.91.0

7.6.3 Determining the dialysis time

After the optimal transfer time has been determined the optimal dialysis time must also be determined, this depends on the total ionic concentration. The dialysis time with the stopped acceptor solution flow must be selected so that 100% of the sample concentration is achieved in the acceptor solution. For the 6.2714.010 Dialysis membrane from Metrohm (cellulose acetate; thickness= 115 µm; pore size= 0.2 µm) the optimal dialysis time is 10 min for a total ionic concentration ≥ 5 mg/L.

Fluorid

Chlori d

Nitri t

Bromid

Nitrat

Phosphat

Sulfat

Transferzeit [min]

If a different dialysis membrane is used or if a total ionic concentration < 5 mg/L is measured the optimal dialysis time must be determined by measuring the recovery rate as a function of the dialysis time. Proceed as follows:

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

7.6 Optimizing the dialysis

1 Measure standard directly

• Immerse the aspiration tubing 16 of the acceptor solution in

the required ionic standard. This should have approximately the same total ionic concentration as the sample.

• Start a determination in «IC Net» to measure the standard

directly; the program could look like that shown below:

Not for dialysis without suppression

• Immerse acceptor solution

aspiration tubing 16 (see Fig.

21)in the acceptor solution again and rinse the acceptor channel for approx. 2 min.

• Switch pump of the 833 IC Liquid Handling Dialysis Unit off.

2 Dialyze the standard and measure it

• Set the dialysis time to 5 min in the program (see

Section 7.3.1/7.3.2).

• Immerse sample

aspiration tubing 16 in the standard used in

item 1.

• Start the determination in IC Net and wait until the

chromatogram has been evaluated.

3 Further measurements

• Increase the transfer time in the program (see

Section 7.3.1/7.3.2) in steps of 5 min until the measured values are constant.

• Carry out measurements as described in item 2.

4 Determine the optimal dialysis time

• Plot the relationship between the measured peak areas or

concentrations as a function of the dialysis time (i.e. the recovery rate) and determine the optimal dialysis time.

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

7 833 IC Liquid Handling Dialysis Unit

7.7 Dialysis procedure

For determinations of samples by using dialysis it is advisable to proceed in the following sequence:

1 Prepare acceptor solution

• To avoid interference from air bubbles in the acceptor

channel the ultrapure water used for the acceptor solution should always be degassed for at least 10 min by vacuum, N

or He.

2 Prepare sample

• In order to avoid blocking the sample channel, samples

containing a large amount of suspended or solid particles should always be centrifuged using a benchtop centrifuge at 10'000 min

3 Start up IC system

• Switch on all instruments.

• Start the IC Net software and load/create the required system

(see «IC Net» Instructions for Use).

• Condition the IC column (see 819/820 Instructions for Use).

-1

for 5 min.

4 Start up dialysis system

• Immerse both pieces of aspiration tubing 16 in the acceptor

solution.

• Start the peristaltic pumps in «IC Net» by setting the remote

line 1 (833 Pump Unit) and remote line 2 (833 Dialysis Unit) in the window of the 819 Detector.

• Rinse the dialysis system with acceptor solution for approx.

10 min and then switch off the pump again.

5 Calibration

• Immerse sample aspiration tubing 16 in the standard

solution.

• Start the determination in IC Net and wait until the standard

chromatogram has been evaluated and the next standard can be measured.

6 Sample determination

• Immerse sample aspiration tubing 16 in the sample solution.

• Start the determination in IC Net and wait until the

chromatogram has been evaluated.

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

7.7 Dialysis procedure

7 Rinse dialysis system

• At the end of the measurements immerse sample aspiration

tubing 16 in the acceptor

solution.

• Start the peristaltic pumps in «IC Net» by setting the remote

line 1 (833 Pump Unit) and remote line 2 (833 Dialysis Unit) in the window of the 819 Detector.

• Rinse the dialysis system with acceptor solution for approx.

10 min and then switch off the pump again.

8 Closing down the dialysis system

• To shut down the dialysis cell the acceptor and sample

channels must be rinsed with ultrapure water for approx. 10 min. The inlet and outlet tubing is then screwed off from the dialysis cell and openings 49, 50, 51 and 52 (see Fig. 15) are each closed with a 6.2744.060 Blank stopper.

• If the dialysis system is not to be used for a long time then the

dialysis membrane must be removed and the cell has to be cleaned, see Section 9.2.7.1 and Fig. 15.

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

8 833 IC Liquid Handling Ultrafiltration Unit

8 833 IC Liquid

Handling Ultrafiltration Unit

This version consists of the basic 833 IC Liquid Handling Unit and the

6.2729.110 Filtration Cell.

70 69 68 67 66

71 74 73 72

Fig. 22: 6.2729.110 Ultrafiltration cell

6.2729.100 Ultrafiltration cell

Upper part of ultrafiltration cell

E.301.0111 Sealing ring

Lower part of ultrafiltration cell

V.022.6030 Screw with 4.754.4090

Washer

Outlet for filtrate

Filtration membrane

(e.g. 6.2714.020)

Inlet for sample solution

Outlet for sample solution

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

8.2 Assembling the ultrafiltration cell

This section describes the initial assembly of the ultrafiltration cell. Before the ultrafiltration cell is used a filtration membrane must be inserted. Proceed as follows (see Fig. 22):

1 Prepare ultrafiltration cell

• Remove ultrafiltration cell 66 (6.2729.100) from the packaging

and remove the three screwed-in 6.2744.060 Blank stoppers .

• Use the 6.2621.070 Allen key to loosen the 5 screws 70

completely. Separate lower part 69 from upper part 67 and remove sealing ring 68.

2 Clean ultrafiltration cell

• Thoroughly the clean sealing ring 68, upper part 67 and

lower part 69 of the ultrafiltration cell with ultrapure water and dry with N

Only ultrapure water or ethanol should be used for cleaning the dialysis cell, other organic solvents (e.g. acetone) will damage the Plexiglas cell!

or a lint-free tissue.

3 Prepare filtration membrane

• Use the 6.2831.010 Tweezers to remove a new filtration

membrane 72 (e.g. 6.2714.020) from the packaging and immerse in a Petri dish filled with ultrapure water for approx. 2 min until the membrane is thoroughly soaked with water.

4 Insert filtration membrane

• Place upper part 67 on a paper tissue with its inner side

uppermost.

• Place sealing ring 68 in the recess provided for it in upper

part 67.

• Use the 6.2831.010 Tweezers to place the wet filtration

membrane 72 (e.g. 6.2714.010) inside sealing ring 68 on upper part 67.

Make sure that the filtration membrane soaked with water does not dry out before insertion as otherwise it cannot be used !

5 Close ultrafiltration cell

• Place lower part 69 on upper part 67 so that the two parts are

properly aligned with each other.

• Use the 6.2621.070 Allen key to screw in the 5 screws 70

completely and tighten them up well.

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

8 833 IC Liquid Handling Ultrafiltration Unit

6 Assemble ultrafiltration cell

• Slide 6.2057.020 Cell holder of ultrafiltration cell 66 into a free

holding guide 58 Separation Center.

• Insert the screwed-together ultrafiltration cell 66 in its

6.2057.020 Cell holder so that the heads of the screws 70 are located in the opening provided for them in the holder.

Fig. 23 Inserting the ultrafiltration cell in the holder

in the column compartment of the IC

8.3 Connect filtration cell

To connect filtration cell 66 to the IC system proceed as follows (see also Fig. 24):

Pump tubing

1 Connect pump tubing to the 833 Liquid Handling

Unit

• Attach the two pieces of pump tubing 6.1826.030 (orange-

yellow stopper) and 6.1826.070 (yellow-yellow stopper) as

described in Section 3.2, see Fig. 7.

2 Connect pump tubing for sample

• Screw 6.1803.070 PTFE capillary 77 (23 in Fig. 7) onto

PEEK coupling 21 (6.2744.160) at the delivery side of pump tubing 75 with the yellow-yellow stoppers (6.1826.070) using a PEEK compression fitting 17 (6.2744.010) (see Fig.

7).

• Attach one end of aspiration capillary 16 (6.1803.080) to

PEEK coupling 18 on the suction side of the yellow-yellow pump tubing 75 using a PEEK compression fitting 17 (6.2744.010) (see Fig. 7).

• Immerse the other end of aspiration capillary 16 in a

container with sample solution and fix it in position.

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

8.3 Connect filtration cell

3 Sample feed to filtration cell

• Lead the other end of PTFE capillary 77 through one of the

openings at the front of the 820 IC Separation Center into the column compartment.

• Attach this end of the PTFE capillary to inlet opening 73 on

the base of the ultrafiltration cell using a PVDF compression fitting 64 (see Fig. 22).

4 Tubing connection filtration cell – waste

• Attach one end of PTFE capillary 78 to outlet opening 74 on

the base of the ultrafiltration cell with a PVDF compression fitting 64 (see Fig. 22).

• Lead the other end of PTFE capillary 77 out through opening

on the rear panel of the 820 IC Separation Center and into a waste bottle (e.g. optional: 6.1608.070 Bottle with 6.1602.150 GL45 bottle attachment).

820

Column

Eluent

833

Sample

Fig. 24: Tubing connection system

Filtrat

79 64

66 78

Waste

6.1803.080 PTFE capillary

for sample solution feed

6.2744.010 PEEK compression

fitting

18 6.2744.034 Coupling

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

6.2744.160 PEEK coupling with

tubing security device

6.2744.000 PVDF compression

fitting

66 6.2729.110 Filtration cell

8 833 IC Liquid Handling Ultrafiltration Unit

6.1826.070 Pump tubing

(19 in Fig. 7) with yellow-yellow stoppers for transferring the sample

6.1826.030 Pump tubing

(19 in Fig. 7)with orange-yellow stoppers for transferring the filtrate

6.1803.070 PTFE capillary

(23 in Fig. 7) connection pump tubing – filtration cell (inlet) for transferring the sample

6.1803.080 PTFE capillary

connection filtration cell – waste

Use only the above-mentioned 6.2744.000 PVDF compression fittings for the ultrafiltration cell connections. If 6.2744.010 PEEK

compression fittings are used then stress cracks could occur in the ultrafiltration cell !

5 Transferring the filtrate

Connection filtration cell – pump tubing

• Attach one end of PTFE capillary 79 to the outlet opening for

• Screw this end onto PEEK coupling 18 on the suction

6.1803.050 PTFE capillary

(23 in Fig. 7) connection filtration cell (outlet) – pump tubing for transferring the filtrate

6.1831.100 PTFE capillary

connection pump tubing – valve for transferring the filtrate

6.1831.040 PTFE capillary

connection pump tubing – valve for transferring the filtrate

the filtrate 71 on the top of the ultrafiltration cell using a PVDF compression fitting 64 (see Fig. 22) and lead out the other end through one of the openings on the front of the 820 IC Separation Center.

side of

pump tubing 76 with the orange-yellow stoppers (6.1826.030) using a PEEK compression fitting 17 (6.2744.010) (see Fig. 7, Fig. 24).

6 Transferring the filtrate

Connection pump tubing – injection valve

• Screw one end of PEEK capillary 80 onto PEEK coupling 21

(6.2744.034) at the delivery side of pump tubing 76 with the orange-yellow stoppers (6.1826.030) using a PEEK compression fitting 17 (6.2744.010) (see Fig. 7, Fig. 24).

• Lead PEEK capillary 80 through one of the openings 14

the front or side of the 820 IC Separation Center into the column compartment and screw it onto connection “1” of the injection valve instead

of PTFE-aspiration tubing 63 (see

Fig. 21 and Fig. 23 of the 819/820 Instructions for Use) with a PEEK compression fitting 17 (6.2744.010).

• Tighten up the rotary nipple on the inside of connections 22

and 28

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

to fix PEEK capillary 80 in position.

8.3 Connect filtration cell

7 Tubing connection injection valve – waste

• Insert 6.2744.020 Coupling (from the 820 accessories) into

connection 13

• Screw PTFE aspiration tubing 63

Coupling inserted in connection 13

provided for it in the 820 IC Separation Center.

onto the 6.2744.020

and lead it into the waste

bottle.

8 Rinse ultrafiltration cell

• Each time that a new filtration membrane is inserted any air

that may still be contained in the filtration cell or tubing must be removed. This is done by rinsing the cell and all the tubing with e.g. ultrapure water:

• Immerse aspiration tubing 16 (see Fig. 24) in the rinsing

solution (degassed ultrapure water).

• Switch on the peristaltic pump in the «IC Net» software.

• Rinse the filtration system with ultrapure water for approx. 5

min. Check that the same amount of solution emerges from both the waste outlets in the waste bottle.

• Check all tubing from the storage containers to the tubing

cassettes and filtration cell and up to the waste bottle for leaks. If any leaks are found then the corresponding connection must either be tightened up or replaced.

• If any air bubbles remain in the dialysis cell then screw off

PEEK capillary 80 (filtrate) from outlet 71 and the filtration cell and wait until the air bubbles have vanished. Then screw the tubing back onto the filtration cell again.

8 Closing down the filtration cell

• If the filtration cell is not to be used for a long time then it

must be rinsed with ultrapure water for approx. 10 min. The inlet and outlet tubing is then screwed off from the filtration cell and openings 71, 73 and 74 (see Fig. 22) are each closed with a 6.2744.060 Blank stopper.

• If the filtration cell is not to be used for a long time then the

filtration membrane must be removed and the cell cleaned, see Section 9.2.8.1 and Fig. 22.

With 820.0X20 IC Separation Center equipped with two injection valves it is possible to fill both sample loops from the same 833 IC Liquid Handling Ultrafiltration Unit. In this case connection "1" at valve A (sample loop outlet) must be connected to connection "2" of valve B (sample loop inlet) using a 6.1831.040 PEEK capillary (15 cm).

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

8 833 IC Liquid Handling Ultrafiltration Unit

8.4 Filtration

8.4.1 Selection of possible sample types

Each filtration process using a filtration membrane with a small pore size could be subject to a membrane blockage.

The following table lists some types of sample that have been filtered with the 833 IC Liquid Handling Ultrafiltration Unit with the standard

6.2714.020 Filtration membrane (0.15 µm) or a second filter membrane (0.2 µm) and then analyzed on a Metrohm IC system. The concentrations of the following 7 anions were determined: F

, NO

, HPO

, SO

, Cl-, NO

Sample type Pore size

of membrane

Orange juice with fruit pulp 0.15 40

Surface water 0.15 500

Drinking water 0.15 1000

Ground water 0.15 500

Wastewater 1 0.15 1000

Wastewater 2 0.15 130

Wastewater 3 0.15 40

Wastewater 4 0.15 80

NaCl solution (1%) 0.2 5000

Schöninger digestion soln. 0.2 100

Acidic soil extracts 0.2 1000

Aqueous soil extracts 0.2 200

No. of samples

per filter

The given number of samples that can be filtered on a filter membrane without any loss of quality being observed are empirical values. They have been determined at Metrohm AG and by various customers and should be used as an orientation guide for estimating the application of the ultrafiltration cell for sample preparation. These values must be determined individually for each new application.

8.4.2 Filter working life

A reduction in the recovery rate when analyzing standard solutions can be used as a possible indicator for the early recognition of an impending blockage. Ideally these solutions should be made up in the sample matrix being analyzed.

This means that if a large number of samples are to be analyzed then it is advisable to measure standard solutions at regular intervals, for example after every 5th or 10th sample for sample with a high particle load. However, it is not possible to make any general prediction about the number of possible filtration processes. The development of the recovery rate with the number of samples may also be subject to large variations. While with one sample matrix the recovery rate may remain

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

8.4 Filtration

stable rate for many samples and then drop sharply, with a different sample matrix it may diminish slowly and continuously.

The time when the filter membrane should be replaced ultimately depends on the sample matrix and the specifications of the analytical method used. In our experience very fine and suspended particles in the sample matrix will block the filter membrane more rapidly than coarse particles, which tend to be carried past the membrane in the sample flow.

Instructions for replacing the filter membrane are given in Section 9.2.8.1.

8.4.3 Filter membrane selection

You can apply existing sample preparation rules to filtration with the 833 IC Liquid Handling Ultrafiltration Unit. If you wish to use a different filter membrane from that supplied as standard then please note that, even if the particle size is known, the selection of a membrane with an appropriate pore size does not automatically produce the required results.

Some investigations have shown that the retention capability of normal filter membranes does not always correspond to their specified pore size. The following table shows the qualitative filtering effect of filter membranes with different nominal pore sizes. The tests were carried out on aqueous solutions containing silica particles with particles sizes

1.5 µm and 5 µm.

Test solutions:

silica particles in water

0.5%, 5 µm 0.15 µm no breakthrough

0.5%, 5 µm 3 µm no breakthrough

0.5%, 5 µm 8 µm no breakthrough

0.5%, 5 µm 10 µm breakthrough 2

0.5%, 5 µm 12 µm no breakthrough

0.5%, 1.5 µm 0.15 µm no breakthrough

0.5%, 1.5 µm 3 µm breakthrough

(1)

Nominal pore size according to information supplied by manufacturer.

(2)

All the membranes came from a single manufacturer except this one.

Pore size

of filter membrane 1

Effect

Please also note that, because of their lack of thickness, the retention capability of filter membranes may be lower than that of thicker filters with the same nominal pore size. This should be taken into account when choosing a suitable filter membrane.

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

9 Troubleshooting - maintenance

9 Troubleshooting -

maintenance

9.1 Faults and their remedies

If difficulties occur when carrying out analyses with the IC system, then it is advisable to search for their causes in the following sequence column → pump → eluent → IC system. An overview of faults, their possible causes and remedies can be found in the Instruction for Use of both the 761 Compact IC (Section 5.3) and the 819/820 Modular IC System (Section 4.3.2).

In addition to these general faults, the following table lists those faults that could occur during the operation of an IC Liquid Handling Unit.

Fault Cause Remedy

Inadequate or no supply at all from pump

• Contact pressure too low

• Pump tubing faulty

• 6.2821.120 PEEK filter unit

blocked

• Connection blocked

Suppressor module / Sample preparation module

• Actuator rotor blocked

• Set contact pressure correctly: first press

contact lever 5 on the tubing cassette down as far as it will go, then up again until the solution is just aspirated. Then press the contact lever up by 1 click to achieve the optimal contact pressure.

• Replace pump tubing

(see Section 9.2.4)

• Replace 6.2821.130 filter (see

connection description, Section 9.2.5)

• Check tubing and connections step by

step and clean or replace as necessary. If the suppressor inlets or outlets are blocked then dismantle the suppressor and clean it (see Section 9.2.6.2).

• Replace actuator rotor

(see Section 9.2.6.3).

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

9.1 Faults and their remedies

Fault Cause Remedy

Inadequate or no supply at all from pump

Leaks • Tubing nipple leaks • Tighten up or replace tubing nipples.

Air bubbles in pump circulation system

Dialysis cell

• Dialysis cell inlets blocked

• Sample tubing blocked by too

large particles

• Bacterial growth in sample

channel and dialysis cell

• Narrowed PTFE tubing by

compression fittings tightened too much

Filtration cell

• Filter membrane blocked,

filtration cell inlets blocked

• Narrowed PTFE tubing by

compression fittings tightened too much

• Aspiration tubing not immersed

• Tubing nipple leaks

Dialysis cell

• Acceptor not properly

degassed

• Standing air bubbles

• Replace dialysis membrane and clean

the cell (see Section 9.2.7.1).

• Replace blocked tubing, always

centrifuge sample (see Section 9.2.4).

• Replace tubing16, 57 und 58 for sample

channel regularly, replace dialysis membrane

• Use capillary cutter to cut off narrowed

tubing ends or replace tubing.

• Replace filter membrane and clean the

cell (see Section 9.2.8.1).

• Use capillary cutter to cut off narrowed

tubing ends or replace tubing.

• Completely immerse aspiration tubing.

• Tighten up or replace tubing nipples.

Dialysis cell

• Degas acceptor solution again.

• Small air bubbles do not interfere. For

larger air bubbles rinse the sample channel with degassed acceptor solution (possibly open outlet briefly).

Reduced phosphate sensitivity and/or large baseline increase (suppressor)

Suppressor module / Sample preparation module switches to next position, but does not work properly

• Suppressor capacity reduced

by heavy metal load or organic contaminants

• Suppressor module/Sample

preparation module dry

• Actuator rotor temporarily in

wrong position

• Actuator step not set correctly

• Regenerate suppressor (see Section

9.2.6.1) or replace it (see Section 9.2.6.3).

• Rinse all 3 actuator units with solution for

at least 10 min.

• Switch instrument off and on again.

Activate suppressor with <STEP>. Check that actuator rotor is in correct position (see Section 9.2.6.3). Repeat process 2-3 times, before each switch to next position with <STEP> wait at least 10 s. If necessary set actuator step again (see below).

• Readjust actuator step

(see Section 9.2.6.3).

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

9 Troubleshooting - maintenance

Fault Cause Remedy

Suppressor module / Sample preparation module do not switch to next position

Unsatisfactory yield for dialysis

• Connection to suppressor

module / sample preparation module interrupted

• Suppressor module/Sample

preparation module dry

• Actuator rotor temporarily

blocked

• Actuator dirty

• Actuator has mechanical fault

• Transfer time not determined

correctly

• Dialysis time too short (e.g. at

too low concentration)

• Dry or damaged dialysis

membrane

• Deposits on dialysis

membrane, recognizable by discoloration at sample inlet

• Unsuitable dialysis membrane

• Check cable connection from suppressor

module / sample preparation module to 833 IC Liquid Handling Unit and from 833 IC Liquid Handling Unit to 830 IC Interface / 819 IC Detector.

• Rinse all 3 suppressor units with solution

for at least 10 min.

• Switch instrument off and on again.

• Clean actuator (see Section 9.2.6.2).

• Replace actuator (see Section 9.2.6.3).

• Check optimal transfer time (see Section

7.6.2).

• Check optimal dialysis time (see Section

7.6.3).

• Replace dialysis membrane

(see Section 9.2.7.1).

• Replace dialysis membrane

(see Section 9.2.7.1).

• Use different dialysis membrane.

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

9.2 Care and maintenance

9.2.1 Instrument care

The 833 IC Liquid Handling Unit and its associated modules require a reasonable amount of care. If the instrument becomes excessively dirty this could affect the functioning and shorten the working life of the basically robust mechanism and electronics.

Split chemicals and solvents should be cleaned up immediately. Above all, the connection strip (the mains plug in particular) must be kept clean.

Although this prevented to a large extent by constructive measures, if aggressive media should penetrate the interior of the instrument then the mains plug of the 833 IC Liquid Handling Unit should be pulled out immediately in order to prevent massive damage to the electronics. If such damage should occur please contact the Metrohm service department.

The instrument must not be opened by untrained personnel. Please observe the safety information given in Section 1.4.

9.2.2 Maintenance by Metrohm service

Servicing the 833 IC Liquid Handling Unit should be carried out within the framework of an annual service visit by technicians from Metrohm. If aggressive or corrosive chemicals are used then shorter service intervals are necessary.

The Metrohm service department is always pleased to provide competent advice about the servicing and maintenance of all Metrohm instruments.

9.2.3 Shut down

Suppressor module/Sample preparation module

If the IC system is not to be used for a long time then the whole IC system (without module) must be rinsed salt-free with methanol/water (1:4) to prevent eluent salts from crystallizing out and causing subsequent damage. Rinsing is carried out by disconnecting the column and suppressor and connecting the injector directly to the detector. Rinsing is carried out with methanol/water (1:4) until the conductivity falls below 10 µS/cm.

column and suppressor module/sample preparation

Each of the three suppressor units is rinsed with ultrapure water for approx. 5 min.

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

9 Troubleshooting - maintenance

Dialysis cell

To shut down the dialysis cell the acceptor and sample channels must be rinsed with ultrapure water for approx. 10 min. The inlet and outlet tubing is then screwed off from the dialysis cell and openings 49, 50, 51 and 52 (see Fig. 15) are each closed with a 6.2744.060 Blank stopper.

If the dialysis system is not to be used for a long time then the dialysis membrane must be removed and the cell has to be cleaned, see Section 9.2.7.1 and Fig. 15.

Filtration cell

If the filtration cell is not to be used for a long time then must be rinsed with ultrapure water for approx. 10 min. The inlet and outlet tubing is then screwed off from the filtration cell and openings 71, 73 and 74 (see Fig. 22) are each closed with a 6.2744.060 Blank stopper.

9.2.4 Replacing the pump tubing

The pump tubing is a consumable with a limited working life, which is why it should be replaced at regular intervals (approx. every 2 weeks for continuous use).

The working life of the pump tubing depends primarily on the contact pressure. This is why you should set the contact pressure correctly as described in Section 3.2 and lift up the tubing cassettes completely when the pump is switched off for a long time releasing spring lever 7 on the right-hand side (this means that the optimally set contact pressure is retained).

As the pump always operates with the same direction of rotation this means that the supplied 6.1826.0X0 Pump tubing can be used on both sides. The pump tubing is replaced as follows:

1 Remove old pump tubing

• Press contact lever 5 on the tubing cassette down as far as it

will go.

• Loosen tubing cassette 4 from holding clip 6 by pressing

down spring lever 7 and unhinge it from the holding pin 2 on the 833 IC Liquid Handling Unit (see Fig. 1).

• Remove the old pump tubing.

2 Insert new pump tubing

• Insert new pump tubing 19 (6.1826.0X0) in the tubing

cassette as shown in Fig. 7. Stopper 20 must click into position in the corresponding holder on the left-hand side of the tubing cassette.

• Hinge the tubing cassettes on holding pin and press down

on the right-hand side until spring lever clicks into position in holding clip 6. Take care that the pump tubing does not kink.

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

9.2 Care and maintenance

3 Set the contact pressure

• Press contact lever 5 until the solution is just aspirated. Then

press the contact lever up by 1 further click to achieve the optimum contact pressure.

9.2.5 Changing the filter

The 6.2821.120 Filter unit PEEK 22 (see Fig. 25) serves to avoid contamination by abrasive particles of the pump tubings. The filter unit consists of the housing 82, the filter 83 and the connector 84 to be screwed into the housing 82. For the connection of capillaries PEEK compression fittings 17 (6.2744.010) must be used.

New filter 83 are available as an option with the ordering number

6.2821.130 (10 pieces).

To change the filter 83 dismantle the Filter unit PEEK 22 according to Fig. 25, replace the filter 83 and put it together again. Install the Filter unit PEEK 22 according to Fig. 7 in the flow path again.

For the connection of the filter unit, please note the flow direction arrow printed on the housing.

The filter unit is filled with isopropanol when new. Rinse your IC system carefully after the first installation of a new filter unit.

17 16 17 84 83 82 23

Fig. 25: Filter unit PEEK 6.2821.120

6.1803.0X0 Aspiration

tube/capillary

PTFE tubing/capillary, depends on version, see Section 10.2 Standard

equipment

6.2744.010 PEEK compression

fitting

Discharge capillary

delivery side for connection to: suppressor module sample preparation module dialysis cell ultrafiltration cell

Filter housing

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

Filter 6.2821.130

Filter connector

9 Troubleshooting - maintenance

9.2.6 Suppressor module / Sample preparation module

The 1.753.0010 Suppressor Module and the 1.793.0010 sample preparation module have the same technical construction so their maintenance is described jointly. Wherever the different chemistry requires a different treatment for the modules this is expressly mentioned in the text.

9.2.6.1 Regenerating the actuator units

If the suppressor units of the suppressor module or the cation exchanger units of the sample preparation module come into contact with certain heavy metals (e.g. iron) or organic contaminants for a longer period of time then these can no longer be completely removed with the regeneration solutions normally used (50 mmol/L H mmol/L HClO

). This affects the capacity of the actuator units of the

module. If such capacity problems occur then the actuator units must be treated as follows:

1 Disconnect suppressor module/sample preparation

module from IC system

• Disconnect the module from column and detector.

2SO4

or 50

2 Regenerate suppressor module

• Rinse all 3 actuator units in sequence for approx. 10 min with

one of the following solutions:

Contamination with heavy metals

0.2 mol/L H + 0.1 mol/L oxalic acid (for Fe

2SO4

/Fe+3)

Contamination with organic substances

0.2 mol/L H

/ acetone ≥ 20%

2SO4

Regenerate sample preparation module

• Rinse all 3 actuator units in sequence for approx. 10 min with

one of the following solutions:

Contamination with heavy metals

0.2 mol/L HClO

+ 0.1 mol/L oxalic acid (for Fe2+/Fe+3)

Contamination with organic substances

0.2 mol/L HClO

/ acetone 20%

The 6.1826.050/6.1826.010 Pump tubing consists of PVC and must therefore not be rinsed with solvents that contain acetone. In this case you should either use different pump tubing or use a different pump for rinsing.

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

9.2 Care and maintenance

Connect suppressor module/sample preparation

module to IC system

• Reconnect the module to the IC system. If there are still

capacity problems then the actuator rotor must be replaced (see Section 9.2.6.3).

9.2.6.2 Cleaning the actuator module

Cleaning the suppressor module or sample preparation module may be necessary in the following cases (see also Section 9.1):

• Irreparable blockage of the suppressor

module/sample preparation module (solutions can no longer be transported by the suppressor)

• Irreparable blockage of the actuator of the particular

module (actuator can no longer be switched to next position)

Clean the connection piece and actuator rotor as follows (see Fig. 26):

1 Disconnect suppressor module/sample preparation

module from IC system

• Disconnect the inlet of the suppressor module/sample

preparation module from the column and detector outlet.

2 Dismantle actuator module

• Unscrew sleeve nut 85 from actuator holder 88.

• Pull connection piece 86 and actuator rotor 87 out of actuator

holder 88.

• Loosen connection piece 86 from actuator rotor 87.

3 Clean inlets and outlets

• Connect each of the 6 pieces of capillary tubing attached to

connection piece 86 to the pump in sequence and pump ultrapure water through them.

• Check whether any liquid is escaping from connection piece

86. If one of the inlets or outlets remains blocked then the connection piece must be replaced. Order number 6.2832.010 for suppressor module

6.2835.010 for sample preparation module

4 Clean actuator rotor

• Clean the sealing surface of actuator rotor 87 using a lint-free

cloth and ethanol.

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

9 Troubleshooting - maintenance

5 Insert actuator rotor

• Place actuator rotor 87 in actuator holder 88 so that the

tubing connections on the rear of the rotor fit into the corresponding recesses inside the holder and one of the three holes of the rotor can be seen from below in one of the openings of the holder.

• When the rotor has been correctly inserted its sealing surface

is approx. 4 mm inside the holder. If this is not the case then the rotor must be brought into the correct position from below by using a pointed object (e.g. screwdriver).

8786 85 88

Fig. 26: Actuator assembly

Sleeve nut

Connection piece with inlets and

outlets

6.2832.010 for suppressor module or

6.2835.010 for sample preparation module

6 Clean connection piece

7 Insert connection piece

Actuator rotor

6.2832.000 for suppressor module or

6.2835.000 for sample preparation module

Actuator holder

• Clean the sealing surface of connection piece 86 using a lint-

free cloth and ethanol.

• Insert connection piece 86 in actuator holder 88 so that

connection "1" is at the top and the three connection piece projections fit into the corresponding recesses in the holder.

• Tighten up sleeve nut 85 on the thread of suppressor holder

88 by hand (do not use any tools

833 IC Liquid Handling Unit / Instructions for Use 8.833.1003

9.2 Care and maintenance

8 Connect and condition suppressor module

• Reconnect suppressor module to the IC system (see Section

5.1).

• Before moving the suppressor to the next position for the first

time rinse the 3 actuator units with solution for 5 min.

Connect and condition sample preparation module

• Reconnect sample preparation module to the IC system (see

Section 6.1 and Section 6.2).

• Before moving the suppressor to the next position for the first

time rinse the 3 actuator units with solution for 5 min.

9.2.6.3 Replacing the actuator rotor

It may be necessary to replace actuator rotor 87 contained in the cation exchanger of the suppressor module or sample preparation module in the following cases (see also Section 9.1):

• Irreparable loss of exchanger capacity

(recognizable at suppressor by reduced phosphate sensitivity and/or large increase in baseline)

• Irreparable blockage of the suppressor

(solutions can no longer be transported by the suppressor)

As well as replacing actuator rotor 87 (6.2832.000 in suppressor module, 6.2835.000 in sample preparation module), it may also be necessary to replace connection piece 86 (6.2832.010 in suppressor module, 6.2835.010 in sample preparation module). Exchange these components in the following way (see Fig. 26):

1 Disconnect suppressor module/sample preparation

module from IC system

• Disconnect the inlet of the suppressor module/sample

preparation module from the column and detector outlet.

2 Dismantle actuator module

• Unscrew sleeve nut 85 from actuator holder 88.

• Pull connection piece 86 and actuator rotor 87 out of actuator

holder 88.

• Loosen connection piece 86 from actuator rotor 87.

3 Clean actuator rotor

• Clean the sealing surface of the new actuator rotor 87 using

a lint-free cloth and ethanol.

830 IC Interface / Gebrauchsanweisung 8.830.1001

9 Troubleshooting - maintenance

4 Insert actuator rotor

• Place actuator rotor 87 in actuator holder 88 so that the

tubing connections on the rear of the rotor fit into the corresponding recesses inside the holder and one of the three holes of the rotor can be seen from below in one of the openings of the holder.

• When the rotor has been correctly inserted its sealing surface

is approx. 4 mm inside the holder. If this is not the case then the rotor must be brought into the correct position from below by using a pointed object (e.g. screwdriver)..

5 Clean connection piece

• Clean the sealing surface of connection piece 86 using a lint-

free cloth and ethanol.

6 Insert connection piece

• Insert connection piece 86 in actuator holder 88 so that

connection "1" is at the top and the three connection piece projections fit into the corresponding recesses in the holder.

• Tighten up sleeve nut 85 on the thread of suppressor holder

88 by hand (do not use any tools

7 Connect and condition suppressor module

• Reconnect suppressor module to the IC system (see Section

5.1).

• Before moving the suppressor to the next position for the first

time rinse the 3 actuator units with solution for 5 min.

Connect and condition sample preparation module

• Reconnect sample preparation module to the IC system (see

Section 6.1 and Section 6.2).

• Before moving the suppressor to the next position for the first

time rinse the 3 actuator units with solution for 5 min..

8 Check actuator step

• Check that the actuator rotor moves to the next position as

described in Section 9.2.6.3 and readjust it if necessary.

830 IC Interface / Gebrauchsanweisung 8.830.1001

9.2 Care and maintenance

9.2.6.4 Adjusting the actuator step

It may be necessary to readjust the actuator step on the suppressor module or sample preparation module in the following cases (see also Section 9.2.6.3):

• Suppressor/Sample preparation module does move to

next position but its functions are impaired.

• After replacement of the actuator rotor (see Section

9.2.6.3)

The actuator step is adjusted by using the setting screw Step Adjustment 12 on the rear panel of the 833 IC Liquid Handling Unit.

Proceed as follows:

1 Condition cation exchanger

• If the actuator rotor has been cleaned or replaced the three

cation exchanger units must be conditioned before the actuator rotor is moved to the next position for the first time.

Condition suppressor module

• see Section 5.1.

• Before the suppressor is switched to the next position for the

first time the actuator units should be rinsed with solution for 5 min.

Condition sample preparation module

• See Section 6.1 and Section 6.2.

• Before the sample preparation module is switched to the next

position for the first time the actuator units should be rinsed with solution for 5 min.

2 Check position of actuator rotor

• Switch the instrument off and then on again and activate the

suppressor in «IC Net» with <STEP>.

• By turning the suppressor module or using a mirror check the

position of the actuator rotor as shown in Fig. 27: in one of the openings in the base

of the suppressor module it should be possible to see one of the three holes on the suppressor rotor, at least partially.

• Repeat the process 2-3 times; before each switch to the next

position with <STEP> wait at least 10 s.

• If the rotor stops in an invalid position then the step of the

actuator rotor must be readjusted (continue with item 3).

830 IC Interface / Gebrauchsanweisung 8.830.1001

9 Troubleshooting - maintenance

3 Adjust actuator step

• Turn setting screw 12 as shown in Fig. 27 a little in the

required direction so that the rotor comes to rest in a valid position.

• Activate <STEP> in the software.

• Check the position of the rotor in all 3 possible settings as

shown in Fig. 27.

• Repeat the setting procedure until the rotor is in a valid

position in all of the 3 possible settings. Always wait for at least 10 s before triggering the next STEP command.

opt i malz ul ässi g zul ässi gunzul ässi g unzul ässi g

Fig. 27: Adjusting the actuator step

9.2.7 Dialysis cell

The dialysis membrane is very sensitive to contact and drying out, so avoid touching it with your fingers and ensure that the membrane never dries out when inserted in the cell.

The working life of a dialysis membrane is approx. 1 week if used frequently. It should always be exchanged if there are any indications that the yield has become reduced or that it is being blocked.

Follow the instructions for the installation of the dialysis cell (Section 7.4 and 7.5), its shut down (Section 9.2.3) and for replacement of the dialysis membrane (Section 9.2.7.1).

830 IC Interface / Gebrauchsanweisung 8.830.1001

9.2 Care and maintenance

9.2.7.1 Replacing the dialysis membrane

It may be necessary to replace the dialysis membrane in the following circumstances (see also Section 9.1):

• Reduced yield after dialysis

• Membrane damaged by drying out or deposits or

bacterial growth

• Irreparable blockage of sample channel (sample can

no longer be transported through dialysis cell)

Proceed as follows when replacing the membrane (see Fig. 15):

1 Dismantle dialysis cell

• Screw off the four inlets and outlets of dialysis cell 42 and

take the cell out of the cell holder.

• Use the 6.2621.070 Allen key to loosen the 5 screws 47 and

separate lower part 46 from upper part 43

• Remove old dialysis membrane 45.

2 Clean dialysis cell, insert dialysis membrane and

reassemble cell

• See Steps 2-6 Section 7.4 Assembling the dialysis cell.

3 Connect dialysis cell

• See dialysis cell Section 7.5.2 Connection of the dialysis

cell.

4 Condition dialysis membrane

9.2.8 Ultrafiltration cell

The perfect condition of the filter membrane used is a necessary requirement for the constant high quality of the analytical results, which is why it must be replaced at regular intervals.

In order to asses the necessity of replacing the membrane please consult Section 8.4.

To replace the filter membrane please proceed as follows (see also Fig. 22 in Section 8.2):

9.2.8.1 Replacing the filter membrane

1 Prepare ultrafiltration cell

• Loosen all capillary connections at ultrafiltration cell 66 by

unscrewing the PVDF compression fittings 64.

• Use the 6.2621.070 Allen key (5 mm) to completely loosen

the 5 screws 70, Separate upper part 67 from lower part 69 and remove sealing ring 72 and the used filter membrane.

2 Clean filtration cell, insert new filter membrane

and reassemble the cell

• See steps 2-6 Section 8.2 Assembling the ultrafiltration cell.

3 Connect filtration cell

• See steps 3-5 Section 8.3 Connect filtration cell.

4 Rinse ultrafiltration cell

• See also step 8 Section 8.3.

Each time that a new filtration membrane is inserted any air that may still be contained in the filtration cell or tubing must be removed. This is done by rinsing the cell and all the tubing with e.g. ultrapure water:

• Immerse aspiration tubing 16 (see Fig. 24) in the rinsing

solution (degassed ultrapure water).

• Switch on the peristaltic pump in the «IC Net» software.

• Rinse the filtration system with ultrapure water for approx. 5

min. Check that the same amount of solution emerges from both the waste outlets in the waste bottle.

• Check all tubing from the storage containers to the tubing

cassettes and filtration cell and up to the waste bottle for leaks. If any leaks are found then the corresponding connection must either be tightened up or replaced.

• If any air bubbles remain in the dialysis cell then screw off

PEEK capillary 80 (filtrate) from outlet 71 and the filtration cell and wait until the air bubbles have vanished. Then screw the tubing back onto the filtration cell again.

830 IC Interface / Gebrauchsanweisung 8.830.1001

10.1 Technical data

10 Appendix

10.1 Technical data

Unless anything to the contrary is mentioned, the published data represent typical values for the 833 IC Liquid Handling Unit at an ambient temperature of 25°C.

10.1.1 Basic instrument: 833 IC Liquid Handling Unit 1.833.0010

Pump

Pump type 2-channel peristaltic pump with

20 min 24 min

Capacity (with water, no counterpressure)

Pressure max. 4 bar (0.4 MPa)

Pumpable liquids Clear liquids with no solid particles

Pump tubing material PVC (Tygon

Mains connection

Voltage 115 V: 100...120 V ± 10 %

Typically with at: pump tubing 20 min

6.1826.010 1.41 mL/min 1.69 mL/min

6.1826.030 0.40 mL/min 0.48 mL/min

6.1826.040 0.75 mL/min 0.90 mL/min

6.1826.050 0.43 mL/min 0.52 mL/min

6.1826.070 2.55 mL/min 3.06 mL/min

230 V: 220...240 V ± 10 % Switched with voltage selection insert in fuse holder (see Section 2.2.1)

-1

(50 Hz)

-1

(60 Hz)



ST), PVC (Tygon LFL), PP

-1

24 min-1

Frequency 50...60 Hz

Power consumption 50 VA

Fuses 5 mm dia., 20 mm long

830 IC Interface / Gebrauchsanweisung 8.830.1001

100…120 V: 0.5 A (slow-blow) 220…240 V: 0.25 A (slow-blow)

10 Appendix

Remote interface 15 for pump

Purpose

Socket

Remote control of pump (on/off)

DIN

Socket occupancy

+5V

Remote interface 14 for actuator

Purpose

Remote control of actuator (switches to next position), input signal

Socket

DIN

Socket occupancy

330

833

+5V

10k

Current flows: on No current flows: off

external

* A requirement for a step to be triggered is that

current flows for at least 10 ms. For a further step to be triggered the current must not previously flow for at least 10 ms.

Interface 13 for actuator module

Purpose

Connection of suppressor module or sample preparation module

Socket

Mini DIN

Safety specification

Construction / Testing As per EN/IEC 61010-1 / UL 3101-1,

Protection class 1, Protection code IP40

Safety information These Instructions for Use contain information

and warnings that must be observed by the user in order to guarantee the safe operation of the instrument.

830 IC Interface / Gebrauchsanweisung 8.830.1001

Metrohm 833IC User Manual

Specifications and Main Features

Frequently Asked Questions

User Manual

Table of contents

List of figures

1.1 Instrument description

1 Introduction

1.1.1 833 IC Liquid Handling Pump Unit

1.1.2 833 IC Liquid Handling Suppressor Unit

1.1.3 833 IC Liquid Handling Sample Preparation Unit

1.1.4 833 IC Liquid Handling Dialysis Unit

1.1.5 833 IC Liquid Handling Ultrafiltration Unit

1.2 Parts and controls

1.3 Information about these Instructions for Use

1.3.1 Arrangement

1.3.2 Notation and pictograms

1.4 Safety information

1.4.1 Electrical safety

1.4.2 General safety rules

2 Installation

2.1 Instrument setup

2.1.1 Packaging

2.1.2 Checks

2.1.3 Location

2.1.4 Arranging the instruments

2.2 Mains connection

2.2.1 Setting the mains voltage

2.2.2 Fuses

2.2.3 Mains cable

2.2.4 Switching the instrument on/off

3 Basic instrument

3.1 Electrical connection

3.1.1 Connecting to 761 Compact IC

3.1.2 Connecting to 819 IC Detector

3.1.3 Connecting to 830 IC Interface

3.2 Assembly the pump tubing

3.3 Operation

3.3.1 Switching the instrument on/off

3.3.2 Program settings

4.1 Connection of the suppressor module

5.1 Connection of the Suppressor module

5.2 Handling the suppressor module

6 833 IC Liquid Handling Sample Preparation Unit

6.1 Connection to modular IC system for neutralization

6.1.1 Electrical connections

6.1.2 Connection of the sample preparation module

6.2 Connection to modular IC system for cation separation

6.2.2 Settings in IC Net

6.3 Handling the sample preparation module

7 833 IC Liquid Handling Dialysis Unit

7.1 Flow diagram for dialysis

7.2 Electrical connection

7.2.1 Dialysis without suppression

7.2.2 Dialysis with suppression

7.3 Settings in IC Net

7.3.1 Dialysis without suppression

7.3.2 Dialysis with suppression

7.4 Assembling the dialysis cell

7.5 Making the capillary connections

7.5.1 Preparing the 820 IC Separation Center

7.5.2 Connection of the dialysis cell

7.6 Optimizing the dialysis

7.6.1 Determining the rinsing time

7.6.2 Determining the transfer time

7.6.3 Determining the dialysis time

7.7 Dialysis procedure

8 833 IC Liquid Handling Ultrafiltration Unit

8.2 Assembling the ultrafiltration cell

8.3 Connect filtration cell

8.4 Filtration

8.4.1 Selection of possible sample types

8.4.2 Filter working life

8.4.3 Filter membrane selection

9 Troubleshooting - maintenance

9.1 Faults and their remedies

9.2 Care and maintenance

9.2.1 Instrument care

9.2.2 Maintenance by Metrohm service

9.2.3 Shut down