Metrohm 844UV-VIS User Manual

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844 UV/VIS Compact IC

Manual

8.844.1053

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

844 UV/VIS Compact IC

Manual

8.844.1053 03.2008 chs

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

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

Documentation in additional languages can be found on

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

tion.

Table of contents

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

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

1.2 Parts and controls .......................................................................................3

1.2.1 Front.................................................................................................................... 3

1.2.2 Rear panel .......................................................................................................... 5

1.2.3 Interior PEEK versions ........................................................................................ 7

1.2.4 Interior Steel versions .........................................................................................9

1.3 Information on the Instructions for Use ...................................................11

1.3.1 Organization .....................................................................................................11

1.3.2 Notation and pictograms.................................................................................. 12

1.4 Safety notes ...............................................................................................13

1.4.1 Electrical safety................................................................................................. 13

1.4.2 General precautionary rules ............................................................................. 13

1.4.3 Recycling and disposal .................................................................................... 13

2 Installation ............................................................... 14

2.1 Overview ....................................................................................................14

2.1.1 Flow chart ......................................................................................................... 14

2.1.2 Connections in the 844 UV/VIS Compact IC.................................................... 15

2.2 Setting up the instrument..........................................................................20

2.2.1 Packaging.........................................................................................................20

2.2.2 Check................................................................................................................ 20

2.2.3 Location ............................................................................................................ 21

2.3 Attaching the accessories.........................................................................21

2.3.1 Connecting the syringe and aspirating tubing................................................. 21

2.3.2 Connecting the drainage tubing for the inner compartment ........................... 21

2.3.3 Connecting PEEK capillaries............................................................................ 21

2.3.4 Connecting Steel capillaries.............................................................................22

2.3.5 Filter unit PEEK ................................................................................................. 23

2.3.6 Filter unit Steel .................................................................................................. 24

2.4 Mains connection ......................................................................................25

2.4.1 Setting the mains voltage................................................................................. 25

2.4.2 Fuses ................................................................................................................ 26

2.4.3 Mains cable and mains connection ................................................................. 26

2.4.4 On/off switching of the instrument ...................................................................27

2.5 Connection to PC ......................................................................................27

2.5.1 Connecting cable .............................................................................................27

2.5.2 Software installation.......................................................................................... 27

2.5.3 First Login ......................................................................................................... 28

2.5.4 Create a system ............................................................................................... 28

2.6 High-pressure pump .................................................................................29

2.6.1 Removing the transport security screws.......................................................... 29

2.6.2 Installing the pulsation dampener.................................................................... 29

2.6.3 Connecting the eluent bottle ............................................................................ 31

2.6.4 Deaerating the pump and rinsing the pulsation dampener............................. 32

2.7 Post column reactor ..................................................................................34

2.7.1 Preparing the peristaltic pump......................................................................... 34

2.7.2 Installation of the post column reactor............................................................. 36

2.7.3 Post column reactor tubing connections ......................................................... 37

2.7.4 Reagent bottle connection ............................................................................... 38

2.8 Columns.....................................................................................................39

844 UV/VIS Compact IC / Gebrauchsanweisung 8.844.1051

Table of contents

2.8.1 Precolumns ...................................................................................................... 39

2.8.2 General information on separating columns ................................................... 40

2.8.3 Connecting the separating column (installation without column heating) ...... 41

2.8.4 Connecting the separating column (installation with column heating) ........... 43

2.9 Detector......................................................................................................48

2.9.1 Installing the flow-through cell ......................................................................... 48

2.9.2 Connect the lamps........................................................................................... 49

2.9.3 Flow-through cell tubing connections.............................................................. 49

2.10 Putting into operation................................................................................50

2.10.1 Putting into operation without post column reactor......................................... 50

2.10.2 Putting into operation with post column reactor.............................................. 52

2.11 Connection of external devices ................................................................55

2.11.1 Connection of the 838 Advanced Sample Processor ..................................... 55

2.11.2 Connection of the 813 Compact Autosampler ................................................ 57

3 Operation .................................................................. 59

3.1 «IC Net» - Terms.........................................................................................59

3.2 Measuring operation .................................................................................59

3.2.1 Opening a system ............................................................................................ 59

3.2.2 Defining measuring channels .......................................................................... 60

3.2.3 Connect a system ............................................................................................ 61

3.2.4 Instrument icon................................................................................................. 62

3.2.5 Hardware start/stop and baseline recording ................................................... 62

3.2.6 Determination start/stop................................................................................... 62

3.3 Settings ......................................................................................................63

3.3.1 Instrument control for connected system ........................................................ 63

3.3.2 Hardware settings ............................................................................................ 70

3.3.3 Spectrum window............................................................................................. 74

4 Notes - Maintenance - Faults ................................... 77

4.1 Practical notes on ion chromatography ...................................................77

4.1.1 Separating columns ......................................................................................... 77

4.1.2 High-pressure pump ........................................................................................ 78

4.1.3 Eluents.............................................................................................................. 78

4.1.4 Peristaltic pump................................................................................................ 79

4.1.5 Connections ..................................................................................................... 79

4.2 Maintenance and servicing .......................................................................80

4.2.1 General information.......................................................................................... 80

4.2.2 Shutdown ......................................................................................................... 80

4.2.3 Changing separating columns......................................................................... 80

4.2.4 Maintenance work at the pump head .............................................................. 82

4.2.5 Replacing the pump tubing ............................................................................. 86

4.2.6 Replacing the UV lamp .................................................................................... 87

4.3 Faults and malfunctions............................................................................89

4.3.1 Error messages ................................................................................................ 89

4.3.2 Malfunctions and their rectification .................................................................. 89

4.4 Quality Management and validation with Metrohm .................................91

5 Appendix ................................................................... 92

5.1 Technical data............................................................................................92

5.1.1 UV/VIS Detector................................................................................................ 92

5.1.2 Injection valve................................................................................................... 93

5.1.3 High-pressure pump ........................................................................................ 93

5.1.4 Peristaltic pump................................................................................................ 94

5.1.5 Leak detector ................................................................................................... 94

Table of contents

5.1.6 Gas Sensor....................................................................................................... 94

5.1.7 RS232 interface ................................................................................................ 94

5.1.8 Remote interface .............................................................................................. 95

5.1.9 Mains connection ............................................................................................. 95

5.1.10 Analog output ...................................................................................................96

5.1.11 Control input .....................................................................................................96

5.1.12 Safety specifications......................................................................................... 96

5.1.13 Electromagnetic compatibility (EMC)............................................................... 96

5.1.14 Temperature control column heating ............................................................... 97

5.1.15 Ambient temperature........................................................................................ 97

5.1.16 Housing ............................................................................................................ 97

5.2 Standard equipment..................................................................................98

5.2.1 PEEK versions .................................................................................................. 98

5.2.2 Steel versions ................................................................................................. 103

5.3 Optional accessories ..............................................................................107

5.3.1 General accessories....................................................................................... 107

5.3.2 High-pressure pump ...................................................................................... 108

5.3.3 High-pressure pump Steel ............................................................................. 109

5.3.4 Separating columns and precolumns............................................................ 110

5.3.5 Communication .............................................................................................. 111

5.3.6 Lamps............................................................................................................. 111

5.4 Warranty and Conformity........................................................................112

5.4.1 Warranty (guarantee)...................................................................................... 112

5.4.2 Declaration of Conformity............................................................................... 113

5.4.3 Quality Management Principles ..................................................................... 114

5.5 Index.........................................................................................................115

844 UV/VIS Compact IC / Gebrauchsanweisung 8.844.1051

III

Table of contents

List of figures

Figure 1: Front 844 UV/VIS Compact IC................................................................... 3

Figure 2: Rear 844 UV/VIS Compact IC.................................................................... 5

Figure 3: Interior PEEK versions ............................................................................... 7

Figure 4: Interior Steel Versions................................................................................ 9

Figure 5: Connecting diagram for 844 UV/VIS Compact IC 2.844.0010 ................ 15

Figure 6: Connecting diagram for 844 UV/VIS Compact IC 2.844.0020 with

Post column reactor ................................................................................

Figure 7: Connecting diagram for 844 UV/VIS Compact IC 2.844.0030 ................ 17

Figure 8: Connecting diagram for 844 UV/VIS Compact IC 2.844.0110 with

Column heating .......................................................................................

Figure 9: Connecting diagram for 844 UV/VIS Compact IC 2.844.0120 with

Post column reactor and Column heating ..............................................

Figure 10: Connecting diagram for 844 UV/VIS Compact IC 2.844.0130 with

Column heating .......................................................................................

Figure 11: Connectors for Steel capillaries............................................................... 23

Figure 12: 6.2821.120 Filter unit PEEK ..................................................................... 24

Figure 13: 6.2620.180 Filter unit Steel ...................................................................... 24

Figure 14: Setting the mains voltage........................................................................ 26

Figure 15: Connection of the pulsation dampener................................................... 30

Figure 16: Connection of eluent bottle ..................................................................... 32

Figure 17: Installing pump tubings ........................................................................... 35

Figure 18: Attaching the post column reactor .......................................................... 37

Figure 19: Post column reactor ................................................................................ 38

Figure 20: Connection of reagent............................................................................. 39

Figure 21: Column connection without column heating........................................... 42

Figure 22: Column heating (closed) ......................................................................... 43

Figure 23: Diagram showing separating column in column heating........................ 44

Figure 24: Installing the column heating................................................................... 47

Figure 25: Flow-through cell installation................................................................... 48

Figure 26: Components of the pump head .............................................................. 83

Figure 27: Replacement of the piston seal 140 ....................................................... 84

Figure 28: Components of inlet valve 141 and outlet valve 142............................. 86

Figure 29: UV lamp (deuterium) ............................................................................... 88

Figure 30: Lamp connections (at the back of the 844 UV/VIS Compact IC) ............ 88

Table of contents

List of numbered parts and controls

1 Door to inner compartment

34 Filter unit PEEK

2 Feedthrough

3 LED "Power"

4 LED "UV"

5 LED "VIS"

6 Connection purge valve

7 Connection for syringe

8 Feedthrough

9 Lamp cooling housing

10 VIS lamp connection

11 UV lamp connection cable

12 UV lamp connection

13 VIS lamp connection cable

14 Analog output

15 Control input

16 USB-B connection

17 USB-A connection

18 RS232 interface

19 Transport security screws

20 Mains switch

21 Mains connection plug

22 Fuse holder

23 Remote interface

24 Connection capillary

25 Connection capillary

26 Magnetic mounting rail for column

heating

27 Pump head

28 Fastening screws

29 Connection capillary

30 Aspirating capillary

31 Connection capillary purge valve

32 Purge valve

33 Connection capillary to syringe

35 Connection capillary

36 Pulsation dampener

37 Leak detector

38 Inlet capillary

39 Drainage tubing connection

40 Mounting pin

41 Aspirating tubing

42 Flow-through cell

43 UV/VIS detector

44 Mounting rail

45 Sample loop

46 Injection valve

47 Column inlet capillary without column

heating

48 Column inlet capillary with column

heating

49 Peristaltic pump

50 Snap-action lever

51 Pump drive

52 Connection capillary steel

53 Connection capillary steel

54 Pump heard steel 6.2824.040

55 Fastening screws steel

56 Connection capillary steel 6.2620.020

57 Purge valve steel

58 Filter unit steel 6.2620.180

59 Connection capillary steel 6.2620.020

60 Injection valve steel

61 UV/VIS detector steel

62 Flow-through cell steel 6.2839.100

63 Sample loop steel 6.2620.110

64 Compression fitting 6.2744.010

65 Compression fitting 6.2744.070

844 UV/VIS Compact IC / Gebrauchsanweisung 8.844.1051

Table of contents

66 Capillary

67 Ferrule (6.2620.010)

68 Ferrule (6.2620.270)

69 Pressure screw (6.2620.000)

70 Steel capillary (6.2620.020)

71 Filter screw of filter unit

72 Filter 6.2821.130

73 Filter housing

74 Steel connection capillary 6.2620.020

75 Steel filter unit 6.2620.180

76 Filter screw of filter unit

77 Filter 6.2620.190

78 Filter housing of filter unit

79 Steel connection capillary 6.2620.020

80 Connection to purge valve

81 Connection to injection valve

82 Aspirating tubing

83 Tubing nipple

84 Threaded stopper

85 Bottle attachment

86 Eluent bottle

87 Aspirating filter

88 CO2 absorber

89 Cotton wool

90 SGJ clip

91 Absorber tube

92 Aspirating tubing for reagent

93 PEEK coupling

94 Pump tubing

95 Stopper (orange-yellow)

96 Tubing cartridge

97 Contact pressure lever

98 Snap-action lever

99 PEEK coupling with filter and tubing

security device

102 PCR holder

103 Connection capillary

104 Post column reactor inlet "eluent in"

105 Post column reactor outlet "to detector"

106 Post column reactor inlet "reagent in"

107 Connection capillary

108 Bottle attachment

109 Supply bottle

110 Steel column inlet capillary

6.2620.160

111 Connection capillary 6.1831.110

112 Steel connection capillary 6.2620.160

113 Separating column

114 Column holder 6.2027.0X0

115 Feedthrough

116 Knurled screw

117 Cover of column heating

118 Connection to 844

119 Magnetic holder

120 Model plate with serial number

121 Feedthrough

122 Connection capillary

123 Connection capillary

124 Steel Connection capillary 6.2620.160

125 Holder plate

126 Capillary prewarming

127 IC Column heating

128 Column heater connection

129 Optical bank

130 Flow-through cell outlet "OUT"

131 Flow-through cell inlet "IN"

132 Knurled screws

133 Screw for piston cartridge

134 Zirconium piston

135 Spring retainer

100 Connection capillary

101 Post column reactor

136 Spring

137 Piston cartridge

Table of contents

138 Piston guide sleeve (4.709.4380)

139 Piston guide sleeve (4.709.4370)

140 Piston seal

141 Inlet valve

142 Outlet valve

143 Screw holder

144 Special tool

145 Special tool

146 Valve housing

147 Sealing ring

148 Sleeve

149 Sapphire sleeve

150 Sapphire sphere

151 Ceramic holder for sapphire sphere

152 Seal

153 UV lamp

154 UV lamp attachment ring

155 Opening for UV lamp

156 Opening for VIS lamp

844 UV/VIS Compact IC / Gebrauchsanweisung 8.844.1051

VII

1.1 Instrument description

1 Introduction

1.1 Instrument description

The 844 UV/VIS Compact IC is a PC-controlled instrument for chromatographic analysis that is available in the six following versions:

• 2.844.0010 UV/VIS Compact IC

• 2.844.0020 UV/VIS Compact IC with post column reactor

• 2.844.0030 UV/VIS Compact IC 844: Steel

• 2.844.0110 UV/VIS Compact IC with column heating

• 2.844.0120 UV/VIS Compact IC with post column reactor

and column heating

• 2.844.0130 UV/VIS Compact IC 844 with column heating: Steel

All the necessary components for chromatography with UV/VIS detection are contained in the extremely compact housing of the 844 UV/VIS Compact IC:

• Injection valve – for single injections or for use with a sample

changer, e.g. the 838 Advanced Sample Processor.

• High-pressure pump – extremely low pulsation double-piston

pump with a flow range of 0.2 … 2.5 mL/min and a maximum pressure of 35 MPa (350 bar).

• Pulsation dampener – the pulsation dampener reliably protects

the columns from damage, even with low-level pressure variations (not necessairy with versions 2.844.0030 and 2.844.0130).

• Column heating – the perfect insulation of the housing creates

thermally stable conditions for the columns (with Versions

2.844.0110, 2.844.0120 and 2.844.0130).

• Columns – whether anion columns, cation columns or separating

columns for organic acids – they all find space in the column compartment of the 844 UV/VIS Compact IC.

• Post column reactor – in the post column reactor the eluate from

the column and a reagent delivered by a peristaltic pump are mixed and transported to the detector. In this way ions that cannot be detected are converted into (optically) detectable species (with Versions 2.844.0020 and 2.844.0120).

• UV/VIS detector – for the determination of transitional metals with

post column derivation, chromate, bromate, nitrite and nitrate in strongly polluted waters, as well as various organic ions.

844 UV/VIS Compact IC / Gebrauchsanweisung 8.844.1051

Table of contents

The two steel versions 2.844.0030 and 2.844.0130 are used for HPLC applications. There is an addittional componet of stel versions:.

• Gas-Sensor – the gas-sensor disrupts power supply, whenever sovent concentration gets too high.

The operation of the 844 UV/VIS Compact IC takes place via a PC connected to the RS232 interface with the help of the «IC Net» control and evaluation program. This PC program can be used to create systems for recording and evaluating chromatograms. Time programs can also be created in which a large number of instrument functions can be triggered for each program step. It is also possible to use programmable signals to control external instruments via the remote interface.

The «IC Net» operating software meets all the requirements you could place today on a modern integration software: single or multi-point calibration, internal or external standard, selectable algorithms for nonlinear calibration, various integration modes with integration parameters and integration events, different methods for peak recognition, peak editor, free scaling, superimposing several chromatograms, use of sample tables and batch reprocessing; a powerful and GLP-conform report generator with output interfaces for monitor, printer and external databases.

The independent «Autodatabase» PC program supplied can be used to save and handle results and chromatograms produced by the «IC Net» program in a database. With «Autodatabase» data can be sorted, filtered and searched with the help of different criteria. In addition, data and curves can be printed out according to user-defined report templates.

The «IC Net» software can be configured and used in order to comply with the Electronic Records and Signatures Rule, known as 21 CFR Part 11, established by the U.S. Food and Drug Administration (FDA). For this purpose the program contains password protection, user administration, electronic signatures, audit trail and administration of methods and results in databases. To use the 21 CFR Part 11 features of

«IC Net» the operating system Windows 2000 or Windows XP with NTFS file system is required.

1.2 Parts and controls

In this Section you will find the numbers and designations of the parts and controls of the 844 UV/VIS Compact IC. The numbering applies throughout the Instructions for Use, i.e. bold numbers in the text (e.g.

) refer to the parts and controls illustrated here.

1.2.1 Front

Figure 1: Front 844 UV/VIS Compact IC

844 UV/VIS Compact IC / Gebrauchsanweisung 8.844.1051

Table of contents

Door to inner compartment

Feedthrough

for eluent, sample, waste, reagent...

LED "Power"

lights up when the instrument is switched on.

LED "UV"

lights up when the UV lamp is on.

LED "VIS"

lights up when the VIS lamp is on.

Connection purge valve

Connection for 6.2816.020 syringe

for aspiration of the sample

Feedthrough

for eluent, sample, waste, reagent...

1.2 Parts and controls

20 19 14

1.2.2 Rear panel

Figure 2: Rear 844 UV/VIS Compact IC

2 Feedthrough

for eluent, sample, waste, reagent...

Lamp cooling housing

VIS lamp connection

for VIS lamp connection cable

UV lamp connection cable

UV lamp connection

for UV lamp connection cable

VIS lamp connection cable

Analog output

output for analog signal

Control input

for control by other instruments

844 UV/VIS Compact IC / Gebrauchsanweisung 8.844.1051

Table of contents

USB-B connection

USB-A connection

RS232 interface

PC connection

Transport security screws

to secure the pump head when the instrument is transported

Mains switch

to switch instrument on and off: I = ON 0 = OFF

Mains connection plug

Mains connection, see Section

Fuse holder

Changing the fuses, see Section

Remote interface

Remote-I/O lines for connection of external devices

2.4

1.2 Parts and controls

1.2.3 Interior PEEK versions

47/48

Figure 3: Interior PEEK versions

844 UV/VIS Compact IC / Gebrauchsanweisung 8.844.1051

Table of contents

Connection capillary

Connection pump head – purge valve, fixed mounting

Connection capillary

in pump head, fixed mounting

Magnetic mounting rail for co-

lumn heating

Pump head (6.2824.100)

Fastening screws

for pump head

Connection capillary

from purge valve to Filter unit PEEK.

6.1831.010 PEEK capillary, length L = 13 cm

Aspirating capillary

Connection for 6.1834.010 aspirating tubing

Connection capillary

from purge valve to connection

Mounting pin

for attaching the tubing cartridges

Aspirating tubing

for sample; PTFE-tubing 6.1803.020

Flow-through cell PEEK

6.2839.130

UV/VIS detector

Mounting rail

for 6.2027.0X0 Column holder, and

6.2057.050 PCR holder

Sample loop

PEEK sample loop

Injection valve

6.1831.110 Column inlet capillary

for column connection without column heating.

6.1831.110 PEEK capillary, length L = 30 cm

Purge valve

Connection capillary to syringe

(with manual injection)

6.1803.020 PTFE tubing, length L = 30 cm

Filter unit PEEK (6.2821.120)

Connection capillary

from Filter unit PEEK to Pulsation dampener.

6.1831.010 PEEK capillary, length L = 13 cm

Pulsation dampener (6.2620.150)

Leak detector

Inlet capillary for injection valve

PEEK capillary 6.1831.010, length L = 24 cm

6.1831.100 Column inlet capillary

for column connection with column heating.

6.1831.100 PEEK capillary, length L = 1 m

Peristaltic pump

for operating the post column reactor

Holding clamp

for locking the tubing cartridge into place

Pump drive

roller head with contact rollers

Connection for drainage tubing

for draining off escaped liquid

1.2 Parts and controls

61 41

1.2.4 Interior Steel versions

Figure 4: Interior Steel Versions

Steel connection capillary

Connection steel pump head – steel

Steel connection capillary

in pump head, fixed mounting

purge valve, fixed mounting

Steel pump head 6.2824.040

844 UV/VIS Compact IC / Gebrauchsanweisung 8.844.1051

Table of contents

Steel fastening screws

for steel pump head

Steel connection capillary

Steel capillary 6.2620.020 from steel purge valve to steel filter unit.

Steel purge valve

Steel filter unit 6.2620.180

Steel connection capillary

Steel capillary 6.2620.020 from Steel filter unit to steel injection valve.

Steel Injection valve

Steel UV/VIS detector

Steel flow-through cell 6.2839.100

Steel sample loop 6.2620.110

1.3 Information on the Instructions for Use

Please read through these Instructions for Use carefully before you put the 844 UV/VIS Compact IC into operation. The Instructions for Use contain information and warnings to which the user must pay attention in order to assure safe operation of the instrument.

1.3.1 Organization

These Instructions for Use 8.844.1053 for the 844 UV/VIS Compact IC provide a comprehensive overview of installation, startup procedure, operation, fault rectification and technical specifications of this instrument. The Instructions for Use are organized as follows:

Sect.

1 Introduction

General description of instrument, parts and controls and safety notes

2 Installation

Sect.

Installation of instrument, accessories, external devices and software

3 Operation

Sect.

Introduction to the operation

4 Notes - Maintenance - Faults

Sect.

Notes on ion chromatography, maintenance, fault rectification, diagnostic tests, validation

Sect.

5 Appendix

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

To find the required information on the instruments, use either the Table of contents or the Index at the back.

As a supplement to the Instructions for Use, the Metrohm Monograph

8.792.5003 "Practical Ion Chromatography" is also supplied. This provides an introduction to the theoretical fundamentals and general information about determinations.

844 UV/VIS Compact IC / Gebrauchsanweisung 8.844.1051

Table of contents

1.3.2 Notation and pictograms

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

Fill Menu item, parameter or entry

value

in the software

SYSTEM STATE Program window

in the software

<OK> Button

in the software

Part or control of 844

Hazard

This symbol draws attention to a possible danger to life or of injury if the associated directions are not followed correctly.

Warning

This symbol draws attention to possible damage to instruments or instrument parts if the associated directions are not followed correctly.

Caution

This symbol marks important information. First read the associated directions before you continue.

Comment This symbol marks additional information and tips.

1.4 Safety notes

1.4.1 Electrical safety

While electrical safety in the handling of the 844 UV/VIS Compact IC is assured in the context of the specifications EN / IEC 61010-1 (protection class should be noted:

• Mains connection

Setting of the mains voltage, checking the mains fuse and the mains connection must be effected in accordance with the

instructions in Section

• Opening the 844 UV/VIS Compact IC

If the 844 UV/VIS Compact IC is connected to the power supply, the instrument must not be opened nor must parts be removed from it, otherwise there is a danger of coming into contact with components which are live. Therefore always disconnect the instrument from all voltage sources before you open it and ensure that the mains cable

is disconnected from mains connection

I, degree of protection IP40), the following points

2.4.

21 !

• Protection against static charges

Electronic components are sensitive to static charging and can be destroyed by discharges. Before you touch any of the components inside the 844 UV/VIS Compact IC, you should ground yourself and any tools you are using by touching a grounded object (e.g. housing of the instrument or a radiator) to eliminate any static charges which exist.

1.4.2 General precautionary rules

• Handling of solvents

Check all lines of the IC system periodically for possible leaks. Follow the relevant instructions regarding the handling of flammable and/or toxic solvents and their disposal.

1.4.3 Recycling and disposal

This product is covered by European Directive 2002/96/EC, WEEE – Waste from Electrical and Electronic Equipment.

The correct disposal of your old equipment will help to prevent negative effects on the environment and public health.

More details about the disposal of your old equipment can be obtained from your local authorities, from waste disposal companies or from your local dealer.

844 UV/VIS Compact IC / Gebrauchsanweisung 8.844.1051

Table of contents

2 Installation

2.1 Overview

2.1.1 Flow chart

The following flow chart provides an overview of all installation work. You will find more detailed information in the relevant Sections.

Setting up sect. 2.2

Installing accessories sect. 2.3

Mains connection sect. 2.4

Connectting PC sect. 2.5

Connecting column

Connecting high press. pump sect. 2.6

Post column reactor?

Precolumn?

Column heating?

sect. 2.8.3

Connecting of the detector sect. 2.9

Conditioning sect. 2.10

Yes

Install post column reactor

Yes

Connecting precolumn sect. 2.8.1

Connecting column and column heating

sect. 2.7

sect. 2.8.4

Connecting external devices sect. 2.11

2.1 Overview

35 36 38 33 41

2.1.2 Connections in the 844 UV/VIS Compact IC

The following illustrations show the internal connections in the 844 UV/VIS Compact IC in schematic form. The meanings of the various numbered components are given in the detailed illustrations and descriptions in Sections

2.2 – 2.11.

Injection valve

113

IC Column

112

UV/VIS

Detector

Eluent

Sample

Waste

Figure 5: Connecting diagram for 844 UV/VIS Compact IC 2.844.0010

844 UV/VIS Compact IC / Gebrauchsanweisung 8.844.1051

Table of contents

94 93

Eluent

Injection

valve

Sample

108

109

IC Column

Reagent

113

103

107

UV/VIS

Detector

Post column

reactor

101

100

Waste

Figure 6: Connecting diagram for 844 UV/VIS Compact IC 2.844.0020 with

Post column reactor

2.1 Overview

Fehl

110 113 112

Figure 7: Connecting diagram for 844 UV/VIS Compact IC 2.844.0030

844 UV/VIS Compact IC / Gebrauchsanweisung 8.844.1051

Table of contents

46 45

Injection

valve

127

Column heating

IC Column

113

122

UV/VIS

Detector

Eluent

Waste

Sample

Figure 8: Connecting diagram for 844 UV/VIS Compact IC 2.844.0110 with

Column heating

2.1 Overview

35 36 33 46 48

UV/VIS

Detector

127

Column heating

IC Column

113

105

104

Post column

reactor

Injection

valve

101

107

108

109

Waste

Eluent

Sample

Reagent

Figure 9: Connecting diagram for 844 UV/VIS Compact IC 2.844.0120 with

Post column reactor and Column heating

844 UV/VIS Compact IC / Gebrauchsanweisung 8.844.1051

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Fehl

110

Column heating

IC Column

113

112

127

Eluent

Sample

Figure 10: Connecting diagram for 844 UV/VIS Compact IC

2.844.0130 with Column heating

2.2 Setting up the instrument

2.2.1 Packaging

The 844 UV/VIS Compact IC is supplied together with the separately packed accessories in special packagings containing shock-absorbing foam linings designed to provide excellent protection. The instrument itself is packed in an evacuated polyethylene bag to prevent the ingress of dust. Please store all these special packagings as only they assure transport of the instrument free from damage.

2.2.2 Check

After receipt, immediately check whether the shipment is complete and has arrived without damage (compare with delivery note and list of accessories in Section structions in Section

5.2). In the case of transport damage, see in-

5.4.1 "Warranty".

2.3 Attaching the accessories

2.2.3 Location

Position the instrument in the laboratory at a location convenient for operation, free from vibrations and protected against a corrosive atmosphere and contamination by chemicals.

To avoid disturbing temperature influences on the insulated column compartment, the instrument must be protected against direct sunlight.

2.3 Attaching the accessories

2.3.1 Connecting the syringe and aspirating tubing

For the manual filling of sample loop 45/63 mounted at the injection valve the 6.2816.020 Syringe and PTFE aspirating tubing connected to the injection valve) are required. These accessories are attached and adjusted as follows:

1 Connecting the syringe

• Remove the plastic stopper from connection 7 on the front

panel of the 844 UV/VIS Compact IC.

• Push 6.2816.020 Syringe(without needle) into connection until it reaches the stop.

2 Pull out the aspirating tubing

• Pull the PTFE aspirating tubing 41 connected to injection

46/61 through feedthrough 7 by hand as far as

valve required.

41 (already

2.3.2 Connecting the drainage tubing for the inner compartment

The 844 UV/VIS Compact IC has a connection 39 on its front panel to allow any escaped liquid to be drained off from the inner compartment. A piece of drainage tubing can be attached to it. Proceed as follows:

1 Connecting the drainage tubing

• Push 6.1816.060 Silicone tubing onto the connection nipple at the bottom right-hand side of the front panel.

2 Lead the drainage tubing into a drain

• Lead the other end of the drainage tubing into a drain and fix it in position.

2.3.3 Connecting PEEK capillaries

With the versions 2.844.0010, 2.844.0020, 2.844.0110 and 2.844.0120, the connections from the high-pressure pump to the detector consist of

6.1831.010 PEEK capillaries (i.d. = 0.25 mm, o.d. = 1/16"), which are connected with either 6.2744.010 PEEK compression fitting (long) or

844 UV/VIS Compact IC / Gebrauchsanweisung 8.844.1051

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6.2744.070 PEEK compression fitting (short). The connection pieces are mounted on the capillaries as follows:

PEEK capillaries that are to be provided with new connection pieces must have a perfectly flat cut surface. This is best achieved by using the 6.2621.080 Capillary cutter available as an option.

1 Mounting the compression fitting

• At the end of capillary Fehler! Verweisquelle konnte nicht gefunden werden. that is to be attached push either a compression fitting Fehler! Verweisquelle konnte nicht gefunden werden. (6.2744.010) or compression fitting Fehler! Verweisquelle konnte nicht gefunden werden. (6.2744.070) over the capillary as shown in Fehler! Verweisquelle konnte nicht gefunden werden..

2 Lead the capillary into the connection

• Push the capillary end into the corresponding connection until it reaches the stop (in order to avoid dead volume).

3 Tighten up compression fitting

• Tighten up compression fitting Fehler! Verweisquelle konnte nicht gefunden werden. or Fehler! Verweisquelle konnte nicht gefunden werden. by hand (do not use any tools).

Figure 11: Connectors for PEEK capillaries

2.3.4 Connecting Steel capillaries

With the versions 2.844.0030 and 2.844.0130, the connections from the high-pressure pump to the detector consist of 6.2620.020 Steel capillaries (i.d. = 0.25 mm, e.d. = connected with the steel connectors 6.2620.010 Ferrule and

6.2620.000 Pressure screw available as an option. The connection pieces are mounted on the capillaries as follows:

Compression fitting

(6.2744.010)

Compression fitting

(6.2744.070)

Capillary 6.1831.XXX PEEK

capillary

/16", length = 3 m), which are

Steel capillaries fitted with new connectors must have a perfectly flat cut surface. This is best achieved by using the 6.2621.040 Capillary tubing cutter available as an option.

2.3 Attaching the accessories

1 Mount connectors

Slide a pressure screw 69 (6.2620.000) and a ferrule 68 (6.2620.010) over the end of the capillary

2 Insert capillary in connection

Push capillary end into the corresponding connection as far as it will go (to avoid dead volume).

3 Tighten pressure screw

Tighten pressure screw 69 with the open-end spanner 1/4" (6.2621.010) supplied.

70 to be fastened.

Figure 11: Connectors for Steel capillaries

2.3.5 Filter unit PEEK

With the versions 2.844.0010, 2.844.0020, 2.844.0110 and

2.844.0120, there is a 6.2821.120 PEEK filter unit mounted between

the high-pressure pump and injection valve against particles.

PEEK filter unit New filters

6.2821.130 (10 pieces).

34 consists of housing 73, filter screw 71 and filter 72.

72 are available as an option under ordering number

Ferrule (6.2620.010)

used in pre-installed components only

Ferrule (6.2620.270)

Pressure screw (6.2620.000)

Capillary

6.2620.020 Steel capillary

46. It protects the valve

When connecting the filter unit please note the flow direction arrow printed on the housing.

844 UV/VIS Compact IC / Gebrauchsanweisung 8.844.1051

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71 72 73

Figure 12: 6.2821.120 Filter unit PEEK

29 Connection capillary

6.1831.010 PEEK capillary, length L = 13 cm

34 Filter unit PEEK (6.2821.120)

35 Connection capillary

6.1831.010 PEEK capillary, length L = 13 cm

2.3.6 Filter unit Steel

With the versions 2.844.0030 and 2.844.0130, there is a Steel filter unit 6.2620.180 mounted between the high-pressure pump and

injection valve. It protects the valve against particles.

The Steel filter unit consists of housing New filters

6.2821.130 (10 pieces).

Filter screw of filter unit

Part of 6.2821.120 Filter unit

Filter 6.2821.130

Part of 6.2821.120 Filter unit

Filter housing of filter unit

Part of 6.2821.120 Filter unit

78, filter screw 76 and filter 77.

77 are available as an option under ordering number

When connecting the filter unit please note the flow direction arrow printed on the housing.

Figure 13: 6.2620.180 Filter unit Steel

2.4 Mains connection

Steel connection capillary

6.2620.020

from steel purge valve to steel filter unit.

Steel filter unit 6.2620.180

Filter screw of filter unit

Part of 6.2620.180 Filter unit

Filter 6.2620.190

Part of 6.2620.180 Filter unit

2.4 Mains connection

Follow the instructions below for connecting to the power supply. If the instrument is operated with a mains voltage set wrongly and/or wrong mains fuse, there is a danger of fire!

Filter housing of filter unit

Part of 6.2620.180 Filter unit

Steel connection capillary

6.2620.020

from steel filter unit to steel pulsation dampener

2.4.1 Setting the mains voltage

Before switching on the 844 UV/VIS Compact IC for the first time, check that the mains voltage set on the instrument matches the local mains voltage. If this is not instrument as follows:

1 Disconnect mains cable

Disconnect mains cable from mains connection plug 21 of the 844 UV/VIS Compact IC.

2 Disconnect mains cable

Using a screwdriver, loosen fuse holder 22 below the mains connection plug

3 Check and change fuse if necessary

Carefully take the fuse installed for the desired mains voltage out of fuse holder fuse in the fuse holder is marked by the white arrow imprinted next to the mains voltage range):

100…120 V 1.6 A (slow-blow)

the case, you must reset the mains voltage on the

21 and take out completely.

22 and check its specifications (the position of the

220…240 V 0.8 A (slow-blow)

4 Insert fuse

Change fuse if necessary and reinsert in fuse holder 22.

5 Install fuse holder

Depending on the desired mains voltage, insert fuse holder 22 in the 844 UV/VIS Compact IC so that the corresponding mains

844 UV/VIS Compact IC / Gebrauchsanweisung 8.844.1051

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voltage range can be read normally and the adjacent white arrow points to the white bar imprinted below the fuse holder.

220 – 240 V

100

120 V

220 - 240 V

Figure 14: Setting the mains voltage

2.4.2 Fuses

100 – 120

20 Mains switch

to switch instrument on and off: I = ON 0 = OFF

21 Mains connection plug

2.4.3

100 - 120 V

220

240 V

Mains connection, see Section

22 Fuse holder

One of the two fuses 1.6 A/slow-blow for 100…120 V or 0.8 A/slow-blow for 220…240 V is installed in fuse holder

22 of the 844 UV/VIS Compact

IC as standard.

Ensure that the instrument is never put into operation with fuses of another type, otherwise there is danger of fire!

When checking or changing fuses proceed as described in Section

2.4.1.

2.4.3 Mains cable and mains connection

Mains cable

The instrument is supplied with one of three mains cables

• 6.2122.020 with plug SEV 12 (Switzerland, …)

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

• 6.2133.070 with plug NEMA 5-15 (USA, …)

which are three-cored and fitted with a plug with a grounding pin. If a different plug has to be fitted, the yellow/green lead (IEC standard) must be connected to protective ground (protection class 1).

Any break in the grounding inside or outside the instrument can make it a hazard!

Mains connection

Plug the mains cable into mains connection plug Compact IC.

21 of the 844 UV/VIS

2.5 Connection to PC

2.4.4 On/off switching of the instrument

The 844 UV/VIS Compact IC is switched on and off using mains switch

20. When the instrument is switched on, the mains pilot lamp 3 lights up.

2.5 Connection to PC

2.5.1 Connecting cable

Always switch off 844 UV/VIS Compact IC and PC before you connect the two instruments with the 6.2134.100 Cable.

Connect the RS232 interface serial COM port at the PC using the 6.2134.100 Cable (9-pin/9-pin). If only a 25-pin COM interface is available on the PC then the 6.2125.110 Adapter cable or a commercially available adapter must be used.

18 at the 844 UV/VIS Compact IC to a

2.5.2 Software installation

The PC program «IC Net» (from Version 2.3 SR2) is required for operating the 844 UV/VIS Compact IC; this is included in the standard equipment on CD 6.6034.033. This program runs under the operating systems Windows 2000 and Windows XP and is installed as follows:

1 Install program

• Insert the installation CD 6.6034.033 into your CD-ROM drive.

• If the autorun option for the CD drive is disabled, select

<Start> and Run. Browse for the Setup.exe file on the

installation CD and click on

• Click "

2 Files

• The installation program copies the files from the installation CD into the folder entered by you and generates the subfolders IC Net and Autodatabase. The following subfolders are also generated, among others:

IC Net" and follow the on-screen prompts of the Setup

program (see Instructions for Use «IC Net», Section 1.5 for a more detailed description).

Data Folder for storage of chromatogram files

Devices Folder for storage of device files (*.dev) Excelreport Folder for Excel reports (*.xls) Methods Folder for storage of method files (*.mtw) Reports Folder for storage of report files (*.txt)

Systems Folder with subfolders with system files

<OK>.

*.chw) and batch reprocessing files (*.bar)

(

and graphic files (

(

*.smt) and sample queue files (*.que).

*.wmf)

844 UV/VIS Compact IC / Gebrauchsanweisung 8.844.1051

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The installed files (incl. system and method files) are generally not write-protected. To prevent these files from being deleted by mistake, switch on the write-protection or make a backup copy in another directory.

2.5.3 First Login

Starting and closing of the Software is described in the provided Software Instructions for Use «IC Net», Section 2.

The

Add User window (see below) opens the first time you launch the

program after installing the software and a user with Administrator access rights is created.

2.5.4 Create a system

Create in «IC Net» a system to control the 844 UV/VIS Compact IC. Proceed as described in Section 4.4.1 of the Software Instructions for Use «IC Net»: System wizard. Add your version of the 844 UV/VIS Compact IC (they are listed under "Metrohm Detectors") to the system, and choose the port to which it is connected.

2.6 High-pressure pump

In order to avoid damage to the pump it must never be operated dry. Each time that the pump is switched on always first check that the eluent supply has been connected up correctly and that sufficient eluent is present in the eluent bottle.

2.6.1 Removing the transport security screws

In order to prevent the pump drive from being damaged during transport the pump head is fitted with three transport security screws

19. These transport security screws must be removed before the highpressure pump is started up. Also remove the red sticker attached to the pump head

In order to avoid damage to the pump head these three security screws should be attached to the pump head each time that the 844 UV/VIS Compact IC is to be transported.

27/54.

2.6.2 Installing the pulsation dampener

With the PEEK versions 2.844.0010, 2.844.0020, 2.844.0110 and

2.844.0120, the 6.2620.150 Pulsation dampener MF has to be

installed between the high-pressure pump and the injection valve of the 844 UV/VIS Compact IC, to protect the column material against pressure drops caused by the injection valve. Proceed as follows:

1 Install pulsation dampener

• Position the pulsation dampener 36 in the interior of the Com-

pact IC on the base.

2 Connection to the pump

• Unscrew PEEK capillary 35 of coupling and attach it to

connection

3 Connection to injection valve

• Unscrew PEEK capillary 38 of coupling and attach it to

connection

The pulsation dampener is filled with isopropanol and must be rinsed with eluent before connection to a separating column (see Section

2.6.4).

80 of the pulsation dampener 36.

81 of the pulsation dampener 36.

The 6.2620.150 Pulsation dampener can be operated in both directions.

The two steel versions 2.844.0030 and 2.844.0130 are operated without Pulsation dampener.

844 UV/VIS Compact IC / Gebrauchsanweisung 8.844.1051

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Figure 15: Connection of the pulsation dampener

29 Connection capillary

6.1831.010 PEEK capillary, length L = 13 cm

32 Purge valve

34 Filter unit PEEK (6.2821.120)

35 Connection capillary

from Filter unit PEEK to Pulsation dampener.

6.1831.010 PEEK capillary, length L = 13 cm

36 Pulsation dampener (6.2620.150)

80 81

38 Inlet capillary for injection valve

PEEK capillary 6.1831.010, length L = 24 cm

46 Injection valve

Connection to purge valve

Connection to injection valve

2.6 High-pressure pump

2.6.3 Connecting the eluent bottle

The eluent supply line from the storage bottle to the high-pressure pump is connected as follows:

Only degassed (with N

, He or vacuum) and microfiltered (0.45 μm

filter) eluents should be used!

The 6.1608.070 Eluent bottle (2 L) supplied is not suitable for vacu- um degassing. Use a pressure-resistant container for this.

Care must be taken that the eluent used is freely miscible with any solvent remaining in the pump head (the pump head leaves the factory filled with either isopropanol or methanol/water). If this is not the case then the pump must first be rinsed with a solvent which is miscible with both the previous eluent and the following eluent (e.g. acetone).

1 Prepare eluent bottle

• Prepare, microfilter (0.45 μm microfilter) and degas (with N2, He, or vacuum) the suitable eluent for the required application and separating column.

• Fill eluent into eluent vessel

86(clear glass, 2 L).

2 Install bottle attachment

• Firmly screw threaded stopper 84 (6.1446.040; part of

6.1602.160) into the smaller threaded opening (M6) of bottle attachment

• Firmly screw aspirating filter

• Pull the other end of aspirating tubing

threaded opening (M8) of bottle attachment

85 (6.1602.105; part of 6.1602.160).

87 onto aspirating tubing 82.

82. through the larger 85 from below.

• Push O-ring (E.301.0021; part of 6.1602.160) over the free end of aspirating tubing attachment

85.

• Push tubing nipple the free end of aspirating tubing red towards bottle attachment larger opening of bottle attachment

• Insert aspirating tubing

82. and move it towards bottle

83 (4.420.4300; part of 6.1602.160) over

82., move it as far as requi-

85 and screw it loosely in the

85.

82. with screwed-on aspirating filter

87 into eluent bottle 86 and screw bottle attachment 85 onto

eluent bottle

• Pull aspirating tubing

86.

82. so far through the opening of tubing

nipple 83 that aspirating filter 87 is touching the bottom of eluent bottle

• Fix aspirating tubing nipple

86.

82. in place by screwing shut tubing

83.

844 UV/VIS Compact IC / Gebrauchsanweisung 8.844.1051

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84 85 86

3 Mount CO2 absorber tube

• First place a piece of cotton wool 89 followed by CO2

absorber

6839.1000) in the large opening of absorber tube

88 (e.g. Merck soda lime pellets with indicator, no.

91 and then

close it with the plastic lid.

• Fasten absorber tube of SGJ clip

90.

91 to bottle attachment 85 with the aid

4 Connect aspirating tubing to pump

• Lead the free end of aspirating tubing 82. through opening 2 into the inner compartment of the 844 UV/VIS Compact IC.

• Pull aspirating tubing

82 sufficiently far into the interior of the

844 UV/VIS Compact IC, cut off to the required length and push at least 5 mm of it onto aspirating capillary

30 of the

high-pressure pump (it may be necessary to use emery paper).

• If necessary, fix aspirating tubing

82 in the required position

in the interior with the aid of the Y.107.0150 self-adhesive strap.

Aspirating tubing (6.1834.010)

Tubing nipple (4.420.4300; M8)

with E.301.0021 O-ring

Threaded stopper (6.1446.040; M6)

Bottle attachment (6.1602.105)

Eluent bottle (6.1608.070)

Aspirating filter (6.2821.090)

CO2 absorber

Cotton wool

SGJ clip (6.2023.020)

Absorber tube (6.1609.000)

Figure 16: Connection of eluent bottle

2.6.4 Deaerating the pump and rinsing the pulsation dampener

The first time that it is started up the high-pressure pump must be deaerated. Proceed as follows:

1 Prepare for deaeration

• Open the rotary knob on purge valve 32 by approx. ½ turn in the counterclockwise direction.

• Remove the plastic stopper from connection

6 on the front

panel of 844 UV/VIS Compact IC.

• Push 6.2816.020 Syringe (without needle) into connection

until the stop is reached.

2.6 High-pressure pump

2 Open and connect system

• Start the «IC Net» PC program, if it has not already been

started (see Section

• Select

File / Open / System in the main window. Select the

system created in Section

2.5.3).

2.5.4, and click on <Open>.

• Select the

Connect to workplace item of the Control menu in this

window.

3 Set flow rate to 2 mL/min

• Double-click the 844 icon in the system window to open the window for manual control of the 844 UV/VIS Compact IC (see below).

• Set the flow rate to

• Click to

<Set> to send this value to the 844 UV/VIS Compact

2 mL/min in the Flow field.

IC.

844 UV/VIS Compact IC / Gebrauchsanweisung 8.844.1051

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4 Deaerate pump

• Make sure that the aspirating tubing 82 for the high-pressure

pump has been immersed into the eluent.

• Click the

<On> button for IC pump to switch on the high-pres-

sure pump.

• Use the syringe inserted into connection

6 to aspirate air until

eluent flows bubble-free into the syringe.

• Click the

<Off> button for IC pump to switch off the high-pres-

sure pump.

• Close the rotary knob on purge valve

32 by turning it in a

clockwise direction.

• Remove the syringe from connection

5 Rinse pulsation dampener

• Place a beaker beneath the column connection capillary 47.

• Click the

pressure pump and rinse the pulsation dampener

<On> button for IC pump to switch on the high-

36 filled

with isopropanol for approx. 10 min with eluent.

• Click the

<Off> button for IC pump to switch off the high-pres-

sure pump.

6 Reduce flow rate

• Reset the original flow rate under Flow (e.g. 0.5 mL/min).

• Click

<Set> to send this value to the 844 UV/VIS Compact IC.

• Click <Save> to save the values.

2.7 Post column reactor

This chapter covers the two versions 2.844.0020 and

2.844.0120.

With versions 2.844.0010, 2.844.0030, 2.844.0110 or

2.844.0130 you can skip this chapter and go directly to Section

2.8.

Instrument versions 2.844.0020 and 2.844.0120 of the 844 UV/VIS Compact IC contain the 6.2836.000 Post column reactor (see Instructions for Use 8.108.1031 Post column reactor).

2.7.1 Preparing the peristaltic pump

Before it is started up, the accessories must be mounted on the peristaltic pump built into the 844 UV/VIS Compact IC Proceed as follows:

1 Remove the tubing cartridge

• Loosen tubing cartridge 96 mounted above pump drive 51 by pressing down snap-action lever 98 from holder clip 50 and remove it from mounting pin

40.

2.7 Post column reactor

2 Attach coupling 93

• At the left-hand end of pump tubing 94 6.1826.320 push on a

coupling

93 6.2744.030. Slightly moistening the Tipp of the

coupling makes this easier.

• Fix "Aspirating tubing for reagent" compression fitting

64 (6.2744.010).

92 to coupling 93 using

3 Attach "Coupling with filter and tubing security

device" 99

• To the right-hand end of pump tubing

94 6.1826.320

attach a "coupling with filter and tubing security device" 99

6.2744.180:

• Dismantle the tubing security device and first push the union nut and compression piece onto the tubing.

• Push the tubing onto the coupling and screw the union nut onto the coupling to secure the tubing.

4 Insert the pump tubing

• Insert the fitted-out pump tubing 94 into the tubing cartridge. The middle stopper

95 should click into position in the

corresponding holder on left-hand side of the tubing cartridge.

5 Reinsert the tubing cartridge

• Insert the tubing cartridge with pump tubing 94 into the front of the holding clip. Insert the left-hand side first, then press down the right-hand side until snap-action lever position. Make sure that the pump tubing has no kinks.

98 clicks into

100

Figure 17: Installing pump tubings

64 Compression fitting (6.2744.010)

Aspirating tubing for reagent

6.1803.020 PTFE tubing

72 Filter 6.2821.130

Coupling (6.2744.030)

844 UV/VIS Compact IC / Gebrauchsanweisung 8.844.1051

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Pump tubing 6.1826.320

for reagent

Stopper (orange-yellow)

Snap-action lever

for releasing the tubing cartridge

PEEK coupling with filter and

tubing security device 6.2744.180

Tubing cartridge (6.2755.000)

Connection capillary

100

Contact pressure lever

for adjusting the contact pressure

PTFE Capillary 6.1803.150, length L = 20 cm

2.7.2 Installation of the post column reactor

The installation procedure is as follows:

1 Attach PCR holder 102

• Push the PCR holder with the strip on its rear panel onto lower mounting rail

2 Insert post column reactor 101 in PCR holder 102

• Insert post column reactor 101 into PCR holder 102 with its tubing connections facing upward.

• Push PCR holder downward as possible.

44.

102 with post column reactor 101 as far

2.7 Post column reactor

101 102

Figure 18: Attaching the post column reactor

49 Peristaltic pump

for operating the post column reactor

6.2836.000 Post column reactor

101

6.2057.050 PCR holder

102

Holder for post column reactor

2.7.3 Post column reactor tubing connections

The connections for the column (Section 2.8) and detector (Section 2.9) are described later. In this first step the reagent flow is connected:

1 Connect pumping tube to inlet "reagent in" 106

• Attach connection capillary 100 6.1803.050 (20 cm) to post

column reactor inlet "reagent in" fitting

64 (6.2744.010).

106 using a compression

844 UV/VIS Compact IC / Gebrauchsanweisung 8.844.1051

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101

104

107

105

103

106

100

100 Connection capillary

PTFE Capillary 6.1803.050, length L = 20 cm

101 Post column reactor 6.2836.000

Connection capillary

103

PEEK Capillary 6.1831.110, length L = 30 cm

Post column reactor "eluent in"

104

Inlet from column

Post column reactor "to detector"

105

Outlet to detector

Post column reactor "reagent in"

106

Inlet for post column reagent from peristaltic pump

107

101

Figure 19: Post column reactor

The post column reactor connections to the column and detector are described in Section

2.8 and Section 2.9.

2.7.4 Reagent bottle connection

The reagent solution tubing from the supply bottle to the peristaltic pump is mounted as follows:

Connection capillary

PEEK Capillary 6.1831.110, length L = 30 cm

If a column heating is used, the capillary

124 is connected here.

1 Preparing the supply bottle for the reagent

• Fill the reagent solution into supply bottle 109 (amber glass, 1 L) and label the bottle.

• Screw bottle attachment

108 onto supply bottle 109.

2 Connect aspirating tubing for reagent

2.8 Columns

• Prepare aspirating tubing 92: cut a piece of 6.1803.020 PTFE

tubing to the required length (normally approx. 120 cm).

• Pull one end of the aspirating tubing compression fitting the tubing projects.

• Screw PEEK compression fitting opening of bottle attachment bottle for the regeneration solution and tighten it up so that the tubing is firmly held.

• Lead the free end of aspirating tubing of the openings 2 of the 844 UV/VIS Compact IC and pull it sufficiently far into the inner compartment.

• Connect aspirating tubing

94 using a compression fitting 64 and a coupling 93.

64 (6.2744.010) so that approx. 30 cm of

108 mounted on the supply

92 to the inlet end of pump tubing

92 through a PEEK

64 with the tubing into one

92 from above into one

Figure 20: Connection of reagent

2.8 Columns

2.8.1 Precolumns

108

109

64 Compression fitting

(6.2744.010)

92 Aspirating tubing for reagent

6.1803.020 PTFE tubing

Bottle attachment

108

(6.1602.150)

Supply bottle 6.1608.020

109

The use of easily exchangeable precolumns protects the separating columns and prolongs their lifetime. The precolumns available from Metrohm are either real precolumns or precolumn cartridges, which are used together with a cartridge holder. For the installation of a precolumn cartridge into the accompanying cartridge holder see the attached leaflet.

The precolumn that is suitable for your separating column can be found in the Metrohm IC Column Catalog which can be obtained from your local Metrohm agency, the data sheet accompanying your separating column, the product information about separating columns that can be found under chromatography products, or let your agency advise you directly.

844 UV/VIS Compact IC / Gebrauchsanweisung 8.844.1051

http://www.metrohm.com, ion

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New IC precolumns are normally filled with solution and sealed at both ends. Before the precolumn is installed in the system, it must be ensured that this solution is freely miscible with the eluent used (check manufacturer's specifications).

1 Connect precolumn

• The precolumn is mounted upstream from the separating column. Use as short a piece of 6.1831.010 PEEK capillary as possible.

• If column heating is used (see Section can also be placed in the inner compartment of the column heating. Use an S-Guard for this. Other precolumns can only be mounted outside the column heating.

When you install the column, always ensure that this is inserted correctly in accordance with the flow direction (if existent) shown.

2 Rinse the precolumn

• Place a beaker beneath outlet capillary.

• Switch on IC Pump in «IC Net» and rinse precolumn for

approx. 10 min with eluent.

• Switch off IC Pump.

2.8.2 General information on separating columns

The precolumn that is suitable for your separating column can be found in the Metrohm IC Column Catalog, the product information about separating columns that can be found under

rohm.com, ion chromatography products, or let your agency advise

you directly.

2.8.4 the precolumn

http://www.met-

New IC separating columns are normally filled with solution and sealed at both ends. Before the column is installed in the system, it must be ensured that this solution is freely miscible with the eluent used (check manufacturer's specifications).

The separating columns currently available from Metrohm and precolumns can be found in the Metrohm IC Column Catalog, or on the Internet under

http://www.metrohm.com in the ion chromatography

product section. Each column is supplied with a test chromatogram and a data sheet. More detailed information about special IC applications can be found in the relevant "Application Bulletins" or "Application Notes"; these are available on the Internet under

http://www.metrohm.com in the applications sector, or can be

requested free of charge from your local Metrohm agency.

When you install the column always ensure that this is inserted correctly in accordance with the flow direction shown.

2.8 Columns

2.8.3 Connecting the separating column (installation without column heating)

This chapter covers the two versions 2.844.0010, 2.844.0020, and

2.844.0030.

With versions 2.844.0110, 2.844.0120, 2.844.0130 you can skip this chapter and go directly to Section

With versions 2.844.0010, 2.844.0020, und 2.844.0030 without column heating the IC separating column is mounted as follows:

1 Connect column to injection valve

• Remove the sealing caps from column 113.

• Without precolumn:

Screw the inlet end of column column inlet capillary compression fitting

• With precolumn:

See accompanying data sheet.

2.8.4.

113 (note flow direction) onto

47/110 at the injector using a

64 (6.2744.010).

2 Rinse column

• Place a beaker under the column outlet.

• Open the software window for manual operation.

• If necessary, set the

Flow rate to a suitable value for the

selected column and send it to the 844 UV/VIS Compact IC with

<Set>.

• Switch on the high-pressure pump (

<On> and rinse the column with eluent for approx. 10 min.

• Switch off the high-pressure pump by clicking on

3 Connect the column outlet

• with 2.844.0010 without post column reactor:

• Connect connection capillary

through cell

42.

111 to inlet "IN" 131 of flow-

• with 2.844.0020 with post column reactor:

• Connect connection capillary

107 to the outlet of column

113 using a compression fitting 64 (6.2744.010).

• Connect connection capillary

107 to the inlet "eluent in" 100

of the post column reactor using a compression fitting 64 (6.2744.010).

IC pump) by clicking on

<Off>.

• with 2.844.0030 without post column reactor:

• Connect steel connection capillary 2.2620.160

“IN”

131 of steel flow-trhough cell 62.

112 to inlet

4 Fastening the column

• Insert one or two column holders 114 (6.2027.030,

6.2027.040 or 6.2027.050) in mounting rail column

844 UV/VIS Compact IC / Gebrauchsanweisung 8.844.1051

113 to the column holder.

44 and attach

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111/ 112/ 107

114

46/ 60

113

47/110

114

Figure 21: Column connection without column

heating

44 Mounting rail

for column holder

104

46 Injection valve

60 Injection valve steel

47 PEEK column inlet capillary

Connecting injection valve column

Steel column inlet capillary

110

113

6.2620.160 from steel injection valve to column

Connection capillary

111

PEEK capillary 6.1831.110, for connection to detector length L = 30 cm

107 Connection capillary

PEEK capillary 6.1831.110, for connection to post column reactor length L = 30 cm

Steel connection capillary

112

6.2620.160 for connection to detector.

46 –

Separating column

113

Column holder 6.2027.0X0

114

2.8 Columns

Bac

2.8.4 Connecting the separating column (installation with column heating)

2.8.4.1 Column heating

Instrument versions 2.844.0110, 2.844.0120 and 2.844.0130 of the 844 UV/VIS Compact IC contain a column heating for thermostatting the separating columns.

115

116

118

119

117

116

Front view

119

120

121

k view

Figure 22: Column heating (closed)

Feedthrough

115

for the capillary from the separating column to detector

Knurled screw

116

for fastening the heater cover

844 UV/VIS Compact IC / Gebrauchsanweisung 8.844.1051

117

Cover of column heating

117

Connection to 844

118

with cable 6.2108.140

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Magnetic holder

119

for fastening the column heater in the

Feedthrough

121

for the column inlet capillary inner compartment of the 844 UV/VIS Compact IC

Model plate with serial number

120

2.8.4.2 Installing a column in the column heating

122/123/124

113

47/110

115

126

116

117

116

Figure 23: Diagram showing separating column in column heating

Column inlet capillary

6.1831.100 PEEK capillary, length L = 100 cm

Steel column inlet capillary

110

6.2620.160 from steel injection valve to column

47/ 110

121

125

Separating column

113

Feedthrough

115

for the capillary from the separating column to detector

Knurled screw

116

for fastening the heater cover

117

2.8 Columns

Cover of column heating

117

Feedthrough

121

for column inlet capillary

Connection capillary

122

47/110

PEEK Capillary 6.1831.120, for the connection to the detector length L = 45 cm

Connection capillary

123

PEEK Capillary 6.1831.120, for the connection to the post column reactor length L = 45 cm

1 Open the column heating

2 Prepare column heating

Connection capillary

124

Steel capillary 6.2620.160, for connection to the detector

Lentth: L=30=cm

Holder plate

125

for separating column

Capillary prewarming

126

for column connection capillary 47/110

• Unscrew the two knurled screws 116 and remove cover 117

from the column heating.

• Lead column inlet capillary 47/110 through feedthrough 121

into the column heating.

• Push column inlet capillary two capillary prewarming slots selected. Push column inlet capillary plate

125 until it appears at the other end.

• Now bend column inlet capillary the inner capillary prewarming slot

47/110 into the outer one of the

126 of the channel you have

47/110 under holder

47/110 and push it through

126 alongside until it

appears at the other end.

• Lead connection capillary reactor) or feedthrough

123 (with post column reactor) outward through

111 using a compression fitting 64 (6.2744.010)

and provide it with a compression fitting

123/124 (without post column

64 6.2744.010 on the

inside.

If not much space is available then the 6.2744.070 PEEK compression fitting short contained in the standard equipment can

also be used for attaching the PEEK capillary.

844 UV/VIS Compact IC / Gebrauchsanweisung 8.844.1051

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3 Insert separating column

• Push column 113 into the holding clips and fasten column

inlet capillary

47/110 to the inlet of the column (bottom) using

a compression fitting 64 6.2744.010.

• with 2.844.0110 without post column reactor:

• Attach capillary

column (top) with a compression fitting

• This will be attached to the detector later (see Section

122 (to the detector) to the outlet of the

64 6.2744.010.

2.9)

• with 2.844.0120 with post column reactor:

• Attach capillary

outlet of the column (top) with a compression fitting

123 (to the post column reactor) to the

6.2744.010.

• This will be attached to inlet "eluent in"

104 of the post

column reactor later (see below, step 6).

4 Close column heating

• Refasten cover 117 onto the column heating using the two

knurled screws

116.

5 Rinse column

• Place a beaker under the eluent flow outlet.

• Open the software window for manual operation.

• If necessary, set the

Flow rate to a suitable value for the

selected column and send it to the 844 UV/VIS Compact IC with

<Set>.

• Switch on the high-pressure pump (

<On> and rinse the column with eluent for approx. 10 min.

IC pump) by clicking on

• Switch off the high-pressure pump by clicking on

6 Connect column to post column reactor

Only with Version 2.844.0120 (with Version 2.844.0110 please go directly to Section

• Attach capillary reactor with a compression fitting

2.8.4.3):

123 to inlet "eluent in" 104 of the post column

64 6.2744.010.

<Off>.

2.8 Columns

2.8.4.3 Installing the column heating

127

128

IC Column heating 1.820.0500

127

Proceed as follows to install the column heating:

1 Insert the column heating

2 Connect column heating

Figure 24: Installing the column heating

Connection for column heating

128

with 6.2108.140 Cable

• Carefully place the column heating inside the 844 UV/VIS Compact IC. Pay attention to the capillaries at feedthroughs 115 and 121 (see Section2.8.4.2).

• Use the magnetic holders

119 to attach the column heating

to their counterparts on the left-hand side inner panel of the 844 UV/VIS Compact IC.

• Plug 6.2108.140 Cable into connection 114 of the column heating and connection

127.

844 UV/VIS Compact IC / Gebrauchsanweisung 8.844.1051

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2.9 Detector

The 844 UV/VIS Compact IC is equipped with UV/VIS detector. The eluent (and the sample) are led through a measuring cell (flow-through cell

42/62) and measured spectroscopically. The available light

sources are a UV (deuterium) lamp and a VIS (halogen) lamp.

2.9.1 Installing the flow-through cell

With the 2.844.0030 und 2.844.0130, the flow-through cell is already pre-installed!

129

Figure 25: Flow-through cell installation

130

132

131

42/ 62

42 6.2839.130 Flow-through cell PEEK

62 6.2839.100 Steel flow-through cell

Optical bank

129

Flow-through cell outlet "OUT"

130

Eluent outlet

To install flow-through cell

1 Remove blank cover

• Optical bank 129 is delivered with a blank cover. This should

be removed.

42/62 proceed as follows:

Flow-through cell inlet "IN"

131

Eluent inlet

Knurled screws

132

For fastening flow-through cell

42/62.

2.9 Detector

2 Attach flow-through cell

• Attach flow-through cell 42/62 to the optical bank with the knurled screws

132.

2.9.2 Connect the lamps

Connect the UV (deuterium) and VIS (halogen) lamps as follows:

1 Connect VIS (halogen) lamp

• Plug "VIS lamp connection cable" 13 into "VIS lamp connection"

2 Connect UV (deuterium) lamp

• Plug "UV lamp connection cable" 11 into "UV lamp connection"

10.

12.

2.9.3 Flow-through cell tubing connections

Make the flow-through tubing connections as follows:

1 Connect flow-through cell inlet

• with 2.844.0010:

• Attach connection capillary

column compression fitting

• with 2.844.0020:

• Attach connection capillary

detector" compression fitting

• Attach the other end of connection capillary (6.1831.110) to inlet "IN" compression fitting 64 (6.2744.010).

• mit 2.844.0030:

• Connection capillary

column through cell

• with 2.844.0110:

• Attach connection capillary

column compression fitting

• with 2.844.0120:

• Attach connection capillary

detector" compression fitting

• Attach the other end of connection capillary (6.1831.120) to inlet "IN" compression fitting 64 (6.2744.010).

113 to inlet "IN" 131 of flow-through cell 42 using a

64 (6.2744.010).

105 of post column reactor 101 using a

64.

112 (6.2620.120) connected to

113 is already connected to inlet „IN“ 131 of flow-

62 at delivery.

113 to inlet "IN" 131 of flow-through cell 42using a

64 (6.2744.010).

105 of post column reactor 101 using a

64.

111 (6.1831.110) connected to

107 (6.1831.110) to outlet "to

131 of flow-through cell 42 using a

122 (6.1831.120) connected to

123 (6.1831.120) to outlet "to

131 of flow-through cell 42 using a

107

123

• with 2.844.0130:

• Attach connection capillary

column

844 UV/VIS Compact IC / Gebrauchsanweisung 8.844.1051

113 to inlet "IN" 131 of flow-through cell 62 using a

124 (6.1831.120) connected to

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pressure screw (6.2620.000) 69.

2 Connect flow-through cell outlet

• with 2.844.0010, 2.844.0030, 2.844.0110 and 2.844.0130:

• Cut a piece of 6.1831.010 PEEK capillary to the required

length and attach one end of it to outlet "OUT" through cell and place the other end in a waste container.

• with 2.844.0020 and 2.844.0120:

• Attach a 6.1831.100 PEEK capillary (100 cm) to the outlet

"OUT" fitting container.

• with 2.844.0030 and 2.844.0130:

• Attach a 6.1831.100 PEEK capillary (100 cm) to the outlet

"OUT" 62 using a compression fitting 64 (6.2744.010), and place the other end in a waste container.

42 using a compression fitting 64 (6.2744.010),

130 of flow-through cell 42/ 62 using a compression

64 (6.2744.010), and place the other end in a waste

130 of flow-through cell 42/

130 of flow-

2.10 Putting into operation

2.10.1 Putting into operation without post column reactor

Before you start injecting sample solutions with Versions 2.844.0010 /

2.844.0030 / 2.844.0110 / 2.844.0130 (without

the whole system must be checked for leaks and conditioned with eluent until a stable baseline has been achieved. Proceed as follows:

When inserting the column always make sure that it is inserted correctly in the flow direction shown on the sticker (the arrow must point in the flow direction).

1 Open and connect system

• Start the «IC Net» PC program, if it has not already been

started.

• Select system file created in Section Compact IC.

File / Open / System in the main window. Open the

2.5.4 for the 844 UV/VIS

post column reactor)

2.10 Putting into operation

• Select the

Connect to workplace item from the Control menu of

the system window.

2 Open control window

• Double-click on the 844 icon in the system window. The control window for manual operation of the 844 UV/VIS Compact IC appears. Open the subtab system parameters (see Section

3.3.1).

Controls and set the

Make sure that the set flow does not exceed the maximum permissible flow for the particular column (see column data sheet).

3 Start system

• Make sure, that the aspirating tubing 82 for the high-pressure pump is immersed in the eluent.

• In the

844 UV/VIS Compact IC / Gebrauchsanweisung 8.844.1051

Control menu in the system window select the item

Startup hardware (Measure baseline). The high-pressure pump

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starts up. If column heating has been selected on the tab

Configuration (see Section 3.3.1) then the column heating will

also start up. The chromatogram window of the set data recorder opens and the baseline(s) are shown continuously.

4 Check for leaks

• Check all the capillaries and their connections from the highpressure pump to the detector block for escaping liquid. If eluent is escaping then the corresponding compression fitting should be tightened or a new connection should be made.

5 Condition system

• Rinse the system with eluent until the desired stability of the baseline is reached (normally 30…60 min; if the eluent is changed, the establishment of the ion exchanger equilibrium on the separating column can take longer).

• The instrument is now ready for sample determinations using the selected system.

2.10.2 Putting into operation with post column reactor

The two Versions IC 2.844.0020 and 2.844.0120 are supplied with post column reactor system must be checked for leaks and conditioned with eluent until a stable baseline has been achieved. Proceed as follows:

When inserting the column always make sure that it is inserted correctly in the flow direction shown on the sticker (the arrow must point in the flow direction).

1 Open and connect system

• Start the «IC Net» PC program, if it has not already been started.

• Select system file created in Section Compact IC.

101. Before sample injection can be done, the whole

File / Open / System in the main window. Open the

2.5.4 for the 844 UV/VIS

2.10 Putting into operation

• Select the Connect to workplace item from the Control menu of the system window.

2 Open control window

• Double-click on the 844 icon in the system window. The control window for manual operation of the 844 UV/VIS Compact IC appears. Open the subtab system parameters (see Chap

3.3.1).

Controls and set the

Make sure that the set flow does not exceed the maximum permissible flow for the particular column (see column data sheet).

3 Start system

• Make sure that aspirating tubing 82 for the high-pressure pump is immersed in the eluent, and that aspirating tubing 108 for the post column reactor is immersed in the reagent.

• In the

Control menu in the system window select the item

Startup hardware (Measure baseline). The high-pressure pump

starts up. If they have been selected on the tab (see Section 3.3.1) then the peristaltic pump and the column heating will also start up. The chromatogram window of the set data recorder opens and the baseline(s) is/are shown continuously.

4 Set contact pressure for pump tubings

• On tubing cartridge 96 press contact pressure lever 97 upward until the reagent solution is aspirated.

• Then press contact pressure lever

97 upward by 1 more click

in order to achieve an optimal contact pressure.

Configuration

844 UV/VIS Compact IC / Gebrauchsanweisung 8.844.1051

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5 Check for leaks

6 Condition system

• The instrument is now ready for sample determinations using the selected system.

Pump tubings are consumable material with a lifetime which depends on the contact pressure. This is why the tubing cartridges should be raised completely by loosening snap-action lever on the right-hand side if the pump is to remain switched off for a considerable length of time (the set contact pressure remains unchanged).

2.11 Connection of external devices

2.11.1 Connection of the 838 Advanced Sample Processor

The 838 Advanced Sample Processor, which is optionally available from Metrohm, is an automatic sampler for ion chromatography. The 838 Advanced Sample Processor (RS232 interface) is connected to the PC. The control programs are drawn up in the «IC Net» software. In order to synchronize program sequences the 838 Advanced Sample Processor and the 844 UV/VIS Compact IC are connected via the

6.2141.190 Remote cable.

Proceed as follows (after the connection of the 844 UV/VIS Compact IC):

1 Electrical connection 838 – PC

• Connect the RS232 interface of the 838 Advanced Sample Processor to a serial COM interface of the PC using a

6.2134.100 Connection cable(9-pin/9-pin).

2 Electrical connection 844 – 838

• Connect Remote connection 23 of the 844 UV/VIS Compact IC and the Remote connection of the 838 Advanced Sample Processors using a 6.2141.190 Cable (see 838 Instructions for Use).

3 Tubing connection 838 – Injection valve

• Screw off aspirating tubing 41 from injection valve 46/60.

• Cut the PEEK capillary tubing mounted on the 838 Advanced

Sample Processor to the required length (so that it can be connected to injection valve

• Pull the free end of the PEEK capillary tubing through one of the openings of the 844 UV/VIS Compact IC and use a

6.2744.010 PEEK Compression fitting to screw it onto injection valve

4 Tubing connection Injection valve – Waste

• Loosen connection capillary 33 from injection valve 46/60 (sample outlet).

• Cut a piece of 6.1831.060 PTFE capillary (sample changer accessory) to the required length, attach it to injection valve 46/60 using a 6.2744.010 PEEK compression fitting and place the other end in a waste container.

46/60.

46/60 of the 844).

844 UV/VIS Compact IC / Gebrauchsanweisung 8.844.1051

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5 Setting up the 844/838 system

• Select File / Open / System in the main window of the «IC Net » software. Open the system for the 844 UV/VIS Compact IC that you have created in Section

2.5.4.

• Add the 838 Advanced Sample Processor to the system (via

Setup / New devices / Install new devices.., see «IC Net»

Instructions for Use, Section 4.4.4):

•

6 Creating a program for the 838

• Open the window with the system settings of the 838 (with a double-click on the 838 icon or via the right-hand mouse key

open).

• Click on the

Program tab. The 838 Advanced Sample Pro-

cessor is controlled by a command sequence on the tab.

• Create a program (see «IC Net» Instructions for Use, Section

6.26.3):

Program

•

• At the command Scan Wait1 the 838 will wait for an

incoming Remote signal on line 3 (defined in the subtab

guration / Scan

). It will receive this Remote signal from a Remote

Confi-

command included in the time program of the 844 (see below). The 844 and 838 are synchronized in this way.

• For more detailed information about the control of the 838 Advanced Sample Processors via «IC Net» please refer to «IC

2.11 Connection of external devices

Net» Software Instructions for Use, Section 6.26.3.

7 Creating a time program for the 844

• Open the window with the system settings of the 844 (with a double-click on the 844 icon or via the right-hand mouse key

open).

• Open the

Program tab.

• Create a time program:

•

• The Remote command sends a signal to the 838 via

Remote line 3. This signal tells the 838 (which is waiting after the Scan command) to continue with its command sequence.

• The two Valve commands switch the injection valve at the 844 to the positions Fill and Inject.

• For more detailed information about the control please refer to Section 3.3.1 or the «IC Net» Software Instructions for Use.

2.11.2 Connection of the 813 Compact Autosampler

The 813 Compact Autosampler, which is optionally available from Metrohm, is an automatic sampler for ion chromatography. The 813 Compact Autosampler (Remote connection) is connected to Remote connection

23 of the 844 UV/VIS Compact IC using the 25-pin

6.2141.130 Remote cable. The control of the 844 UV/VIS Compact IC takes place using Remote commands in the time program of the 844 UV/VIS Compact IC.

Proceed as follows:

1 Electrical connection 844 – 813

• Connect Remote connection 23 of the 844 UV/VIS Compact IC and the Remote connection of the 813 Compact Autosampler using the 6.2141.130 Cable (see 813 Instructions for Use).

2 Tubing connection 813 – Injection valve

• Screw off aspirating tubing 41 from injection valve 46/60.

• Cut the PEEK capillary tubing mounted on the 813 Compact

Autosampler to the required length (so that it can be connected to injection valve

46/60. of the 844).

• Pull the free end of the PEEK capillary tubing through one of

844 UV/VIS Compact IC / Gebrauchsanweisung 8.844.1051

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the openings of the 844 UV/VIS Compact IC and use a

6.2744.010 PEEK Compression fitting to screw it onto injection valve

46/60..

3 Tubing connection Injection valve – Waste

• Loosen connection capillary 33 from injection valve 46/60.

(sample outlet).

• Cut a piece of 6.1831.060 PTFE capillary (sample changer accessory) to the required length, attach it to injection valve 46/60. using a 6.2744.010 PEEK compression fitting and place the other end in a waste container.

4 Setting a method on the 813

• Use the 813 keyboard on the 813 Compact Autosampler to set the required method (see 813 Instructions for Use).

5 Creating a time program for the 844

• In the main window of the «IC Net» software select File / Open /

System. Open the system for the 844 UV/VIS Compact IC that

you have created in Section

2.5.4..

• Open the window with the system settings of the 844 UV/VIS Compact IC (with a double-click on the 844 icon or via the right-hand mouse key

• Open the

Program tab.

open).

• Create a time program:

•

• The Remote command sends a signal to the 813 via

Remote line 3. The function of this signal depends on the method selected at the 813 (see 813 Instructions for Use, Section 3.4).

• The two Valve commands switch the injection valve of the 844 to the positions Fill and Inject.

• For more detailed information about the control please refer to Section 3.3.1 or the «IC Net» Software Instructions for Use.

3.1 «IC Net» - Terms

3 Operation

This Section describes only the most important points concerning the operation of the 844 UV/VIS Compact IC. For further details please refer to the «IC Net» Instructions for Use and to the on-line help in the PC program.

3.1 «IC Net» - Terms

System

In the «IC Net» software a System contains the devices set under Settings for this system, the created time programs, the data acquisition parameters and the methods that have been optimized for a specific separating column and the determination to be carried out with it. Several systems can be defined and saved as system files (

Systems folder (see «IC Net» Software Instructions for Use, Section

the

4). Determinations (single determinations or using a sample table) are started via the system.

*.smt) in

Each system is linked to a method.

Method

A Method contains all the information necessary for data acquisition, integration, peak evaluation and results calculation. It can be re-

garded as being a skeleton chromatogram, i.e. a chromatogram without any data. Methods are saved as method files (

thods folder.

Chromatogram

A chromatogram is the graphical presentation of the elution curve (signal vs. time).

Chromatograms are saved as chromatogram files ( folder. In addition to the measuring data, the chromatogram files also contain the method parameters and system settings used for data acquisition, processing and remote control.

3.2 Measuring operation

3.2.1 Opening a system

*.mtw) in the Me-

*.chw) in the Data

A system window is opened with IC Net / File / Open / System and the selection of the required system file. It contains symbols for Data

recorder devices that have been installed in the system. A system window for a

system with an 844 UV/VIS Compact IC is shown below:

844 UV/VIS Compact IC / Gebrauchsanweisung 8.844.1051

(keyboard), Watch window (screen) and all

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3.2.2 Defining measuring channels

With the 844 UV/VIS Compact IC up to four measuring channels can be recorded simultaneously: Abs.1, Abs.2, Abs.3 and Ch1/Ch2 (three measuring channels for absorption at different wavelengths, as well as the ratio between measuring channel 1 and measuring channel 2). For each measuring channel you should include one data recorder (icon:

) in the system.

Add a data recorder

Proceed as follows to insert a data recorder: Select

New Devices / Install new device..

YOUR SYSTEM

opens. Select Other modules in the upper selection

, the window ADDING DEVICES TO

SYSTEM / Setup /

list:

Select Data recorder in the list and click on

<Add to system>.

The icons for the data recorders are shown in your system window. An example of a system with four measuring channels is shown below:

Via

IC NET / Options / Global preferences you can arrange the data

recorder icons one above the other under

GLOBAL PREFERENCES.

3.2 Measuring operation

Assign data sources

A data source is assigned to each of these data recorders. Click on one of the data recorders with the right-hand mouse key, and select The

RECORDER window opens.

Setup.

Click on the lower

<choose> button. The DATA SOURCE window opens.

Select one of the data sources that has not been previously connected, and draw it on to the right-hand side by keeping the left-hand mouse key pressed down:

Click on

<OK>. The connected data source is shown in the RECORDER

window:

Click on

<OK> and assign a data source to each data recorder.

3.2.3 Connect a system

The selected system must be linked to the workplace for controlling the instrument and starting determination processes. Systems are linked by selecting Instructions for Use «IC Net 2.3», Section 4.3.1).

SYSTEM / Control / Connect to workplace (see also Software

844 UV/VIS Compact IC / Gebrauchsanweisung 8.844.1051

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3.2.4 Instrument icon

When you click with the right mouse button on the instrument icon, you will see the following menu:

Open Opens the window for System Settings.

Hardware

Spectrum window

Unlink Unlink device from the system.

Opens the window for Hardware Settings.

Opens the SPECTRUM WINDOW.

3.2.5 Hardware start/stop and baseline recording

Start

Starting the hardware (by selecting

hardware) on the 844 UV/VIS Compact IC includes starting the high-

pressure pump and, depending on the system start values

hardware

defined on the Configuration tab, starting the UV lamp, the VIS

lamp, and, if present, the column heating and peristaltic pump.

At the same time Recording the measuring signal is started, using the method defined in the system. The measuring signal is recorded independently from the time for the chromatogram set under until either data acquisition is stopped with

acquisition or a new determination is started. Alternatively data recording

can also be interrupted by clicking on window. In this case the user is asked whether the recorded baseline is to be saved or not.

SYSTEM / Control / Startup

SYSTEM / Control / Stop data

in the chromatogram

Startup with

Duration,

Stop

By selecting

SYSTEM / Control / Shutdown hardware the high-pressure

pump, UV lamp, VIS lamp and, if present, the column heating and the peristaltic pump of the 844 UV/VIS Compact IC will be stopped immediately. The current determination and the processing of the active sample table will also be stopped. In addition, the remote output lines will be set to the values defined for the parameter the tab

Outputs in the HARDWARE window.

PowerON values on

3.2.6 Determination start/stop

Start

By selecting the menu item determination is started with the settings of the selected system. At the start the system start values

SYSTEM / Control / Start determination a

Startup with hardware defined for the system

3.3 Settings

(on the tab Configuration) will be set on the 844 UV/VIS Compact IC. Depending on the recording will either be started immediately (for

Start mode setting the time program and data

Start with determination)

or only when the injection valve is switched to the position "INJECT" (for

Start with inject).

Stop

SYSTEM / Control / Stop determination is selected then the current

If determination is stopped. Data recording and the time program are stopped immediately.

Alternatively the determination can also be stopped by clicking on the chromatogram window. In this case the user will always be asked if the recorded baseline is to be saved or not.

3.3 Settings

3.3.1 Instrument control for connected system

A double-click on the device symbol or selecting the menu item Open with the right-hand mouse key opens the window for the system settings. For a connected system the tab

State

Current state

appears on which the current values are shown.

Manual with the subtab Current

Channel 1 abs, mAU Live display of the absorption in channel 1.

Channel 2 abs , mAU Live display of the absorption in channel 2.

Channel 3 abs, mAU Live display of the absorption in channel 3.

Ch1/Ch2 Live display of the absorption ratio of channel 1

and channel 2.

VIS Lamp Live display of the status of the VIS lamp.

UV Lamp Live display of the status of the UV lamp.

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Pump pressure, MPa Displays the currently measured pressure of the

high-pressure pump (units depend on the settings made under

preferences).

Valve Live display of the position of the injection

IC NET / Global

valve.

Remote lines Live display of the status of the 8 remote lines.

Column temp., °C Live display of the temperature in the column

oven.

Controls

On the subtab pressure pump

Controls injection valve 46/60., peristaltic pump 49, high-

27/54, column heating 115 and remote lines can be

manually controlled. In addition, the parameters for the high-pressure pump and column heating temperature can also be set:

Valve Injection valve

<Inject> Switch injection valve to "Inject" position. <Fill> Switch injection valve to "Fill" position.

Peristaltic pump Peristaltic pump

<On> Start peristaltic pump (only enabled, with

versions 2.844.0020 or 2.844.120).

<Off> Stop peristaltic pump (only enabled, with

versions 2.844.0020 or 2.844.120).

IC pump High pressure pump

<On> Start high pressure pump. <Off> Stop high pressure pump. Flow, mL/min Set value for flow rate of IC pump.

Entry range:

0.20 ... 2.50 mL/min

3.3 Settings

Pressure max, MPa Value for maximum switch-off pressure for high-

pressure pump. Once it has been set this value will be monitored, even if there is no connection to the PC (units depend on the settings made under Entry range:

IC NET / Global preferences).

0.0 ... 35.0 MPa

If the

Flow is higher than 1.5 mL/min, the defined

Pressure max must not exceed 25.0 MPa (250 bar).

Pressure min, MPa Value for minimum switch-off pressure for high-

pressure pump. Once it has been set this value will be monitored, even if there is no connection to the PC (units depend on the settings made under Entry range:

Column oven Column oven

<On> Turn column oven on (only enabled, if a column

IC NET / Global preferences).

0.0 ... 35.0 MPa

oven is connected).

<Off> Turn column oven off (only enabled, if a column

oven is connected).

Temperature, °C Set value for temperature in the column oven.

Entry range:

0 ... 75 °C

Detector

Remote lines Set values for remote line settings 1…8.

Selection: 0, 1

On the subtab

Detector the UV/VIS detector 43/61 can be controlled

manually. The parameters for the measurement can also be set:

UV lamp UV lamp

<On> Turn UV lamp on. <Off> Turn UV lamp off.

844 UV/VIS Compact IC / Gebrauchsanweisung 8.844.1051

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VIS lamp VIS lamp

<On> Turn VIS lamp on. <Off> Turn VIS lamp off.

<Zero> Records a new zero spectrum.

The zero spectrum is a reference spectrum. It should be recorded at a time at which there is no sample in the measuring cell. It is used for calculating the absorption spectrum.

<Spectrum> Opens the SPECTRUM window (see Section

3.3.3).

Wavelength, nm Sets the wavelengths at which the

chromatograms are to be recorded (for max. three measuring channels).

Bunching, nm Sets the bunching of the wavelengths defined

above.

Channel 1, nm Measuring channel 1. Channel 2, nm Measuring channel 2. Channel 3, nm Measuring channel 3.

The relationship between an example:

Set values:

An upper and a lower limit for the measured wavelengths of the corresponding measuring channel are calculated from these values. For these calculations the following equation applies: subtract "1" from the the resulting value from/to the

Result: wavelengths between 490 nm (lower limit) and 510 nm (upper limit) will be included in the chromatogram.

Time program

On the program for instrument control can be entered. This program is started automatically as defined in the either at the moment the determination is started (

determination

Wavelength and Bunching is explained by using

Wavelength = 500 nm, Bunching = 21 nm

Bunching value, divide the new value by 2, and subtract/add

Wavelength value.

Program tab of the system settings window a user-defined time

Start mode window (see Section 4.3.3)

Start with

) or at the moment the sample is injected (Start with inject).

3.3 Settings

The

Program tab contains the two following subtabs:

Program

Program Main time program with all program steps. Remote configuration Possibility for creation of user-defined remote

commands.

On the

Program subtab, program steps including time, program

instruction and parameter can be entered.

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 List of program

instructions).

In addition to these predefined instructions, user-defined remote commands can be entered if activated on the

Remote configuration

tab.

Parameter (3rd column) Parameter for program instruction (see List of

program instructions).

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).

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List of program instructions

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

Program subtab:

Remote 0, 1, *, p

Valve Inject, Fill

ICPump on, off

Flow 0.2 ... 2.5 mL/min

Pmax 0.0 ... 35.0 MPa

Pmin 0.0 ... 35.0 MPa

Peristaltic on, off

Wavelength_1..3 190 ... 900 nm

Bunching_1..3 1 ... 101 nm

UV_Lamp on, off

VIS_Lamp on, off

Zero

Record a new zero spectrum.

Set remote output lines 1...8 to the desired values. For entry of the first value, enter

1, 0, p or *. For entry of

the other values, move the cursor in front of the value to be changed and enter

1, 0, p or *.

Switch injection valve to "INJECT" or "FILL" position.

Switch on or off the high-pressure pump.

Set flow rate of the high-pressure pump to the desired value.

Set maximum pressure limit for the high-pressure pump to the desired value.

Set minimum pressure limit for the high-pressure pump to the desired value.

Switch on or off the peristaltic pump.

Set wavelength of the corresponding measuring channel on the desired value.

Set bunching of the corresponding measuring channel on the desired value.

Switch on or off the UV lamp.

Switch on or off the VIS lamp.

Remote configuration

On the

Remote configuration subtab user-defined remote commands can

be defined, which can be inserted into a time program.

3.3 Settings

Name (1st column) User-definable name of the remote command

Start_838).

(e.g.

Remote command (2nd column)

Setting the remote output lines 1…8. Selection:

For entry of the first value, enter

0 (line off, inactive, open) 1 (line on, active, 0 V) p (pulse) * (leave line in current status)

1, 0, p or *. For

entry of the other values, move the cursor in front of the value to be changed and enter

p or *.

<Add> Add new remote command. <Delete> Delete selected remote command. <Activate> Activate the defined remote commands for

1, 0,

insertion into the time program.

Configuration

The

Configuration tab in the system settings window contains

configuration settings for the 844 UV/VIS Compact IC.

Startup with hardware The activated devices will be started with Startup

hardware or at the start of a determination.

UV lamp If this option is switched off the UV lamp will not

be switched on at

Startup hardware or at the start

of a determination.

VIS lamp If this option is switched off the VIS lamp will not

be switched on at

Startup hardware or at the start

of a determination.

Column oven If this option is switched off the column heating

will not be switched on at

Startup hardware or at

the start of a determination.

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Peristaltic pump If this option is switched off the peristaltic pump

will not be switched on at

Startup hardware or at

the start of a determination.

Reference channel Reference channel.

On If this option is switched on the absorption of

the measuring and reference channels will be shown as a comparative value.

Wavelength, nm Sets the wavelength of the reference channel. Bunching, nm Sets bunching for the wavelength defined

above.

Links

Links tab in the window for the system settings serves to select and

The set the COM port (for details see Software Instructions for Use «IC Net

2.3», Section 5.2.4 Links).

3.3.2 Hardware settings

Selection of the Hardware menu item using the right mouse button opens the hardware settings window consisting of the four tabs

Alarm stops, System settings and Detector settings.

Outputs

Outputs tab of the hardware settings window defines remote output

The signals to be set automatically if specific events occur.

Outputs,

3.3 Settings

Event Events for automatic remote signal output:

Inject Switching of the injection valve to the "INJECT"

position.

Fill Switching of the injection valve to the "FILL"

position.

Pump stop (P max/min)

Pump stopped because pressure limits are exceeded.

Hardware error Hardware error detected at the 844 UV/VIS

Compact IC (high-pressure pump, injection valve, or peristaltic pump not working correctly).

Alarm leak detector Internal leak.

PowerOn values Output lines 1… 8 will be set to the values

Pulse length Length of a pulse in ms.

Alarm stops

The for which the instrument is stopped immediately. At an alarm stop, highpressure pump and peristaltic pump are stopped immediately, the running determination and the active sample queue are also stopped.

defined here after the instrument has been switched on or after an emergency stop with

Shutdown hardware.

Selection:

Alarm stops tab of the hardware settings window defines the events

0, 1

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Shutdown hardware after.. Event for alarm stop:

Pump stop Pump stopped because pressure limits are

exceeded.

Hardware error Hardware error detected at the 844 UV/VIS

Compact IC (high pressure pump, injection valve or peristaltic pump not working correctly).

Leak Leak detector has detected solvent in the

instruments interior.

Power on Temporary power failure at the 844 UV/VIS

Compact IC hardware.

System settings

On the tab rate corrections for the high-pressure pump are defined.

Break time, ms Modification of the break time for the injection

System settings break times for the injection valve and flow

valve. Entry range:

1 ... 99 ms

3.3 Settings

Flow correction Factor for correction of the difference bet-

ween displayed and actual flow rate of the high-pressure pump. Range:

0.9 ... 1.25

The correction factor is determined as

follows by measuring the actual flow rate using a graduated cylinder:

Ch1/Ch2 threshold Limit for measuring channel ratio

Threshold, mAU As long as the absorption value(s)

Analog Outputs Settings for analog signal output.

Range, mAU The defined value is equivalent to 1 V

Detector settings

Flow correction =

Measured flow rate

Displayed flow rate

The product of parameter parameter exceed 2.75 mL/min.

Flow (on the tab Controls) must not

Flow correction and

Ch1/Ch2.

from channel 1, channel 2 or both lie beneath the defined Threshold (limit) the value for the Ch1/Ch2 ratio will not be calculated.

for the analog signal output. Entry range: 0.1 ... 2000.0 mAU

On the tab

Detector settings measuring settings are defined.

Detector settings Settings for UV/VIS detector 43/61.

VIS lamp Display of the voltage of the VIS lamp.

844 UV/VIS Compact IC / Gebrauchsanweisung 8.844.1051

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T int, ms Integration time.

Entry range:

T out, s Measuring time per data point.

Entry range:

Data rate Effective measuring time per data point. The

Data rate is the particular whole number multiple

of the value

out

10 ... 254 ms

0.05 ... 2.00 s

T int that is closest to the value T

The measurement of a data point is explained by using an

example:

Set values:

The calculated

int that is closest to the value T out; in our example 7 times 15

T int = 15 ms, T out = 0.1 s

Data rate is 105 ms (the particular multiple of T

ms). This means that the integration will be carried out 7 times (each time for 15 ms) and then averaged to give a data point.

<Optimize> Optimizes T int and adjusts the VIS lamp.

It should be done

• after exchanging a lamp (UV or VIS)

• if parts of the intensity spectrum are in the

overload ( > 60'000 , peaks cut)

• if the maximum of the intensity spectrum of dist. water is too low (below 33'000)

Before clicking <Optimize>, the flow-through cell should be rinsed and filled with dist. water. There must be no air bubbles in the flow-trough cell when clicking

<Optimize>.

Operating hours Operating hours of the lamps.

UV lamp, h Display of the operating hours of the

UV lamp.

<Reset UV lamp> Set operating hours of the UV lamp

to 0. Click it after replacing the UV lamp.

VIS lamp, h Display of the operating hours of the

VIS lamp.

<Reset VIS lamp> Set operating hours of the VIS

lamp to 0. Click it after replacing the

VIS lamp.

3.3.3 Spectrum window

The SPECTRUM WINDOW can be opened with a right-hand mouseclick on the 844 icon and then selecting the menu item

window

, or via the button on the subtab Manual/Detector.

Spectrum

3.3 Settings

A selection can be made from three different spectra, the absorption spectrum, intensity spectrum and the zero spectrum. Please note that each time you click on

<Update> button will be triggered.

Absorption, Intensity or Zero the function of the

<Update> The 844 measures the current intensity spect-

rum and sends it together with the last zero spectrum to have been recorded to <IC Net>. The absorption spectrum is recalculated from these two spectra.

Absorption The absorption (with the units mAU) is given on

the y-axis as a function of the wavelength (xaxis). The absorption values are calculated for all measured wavelengths and shown as spectrum. The calculation formula for the absorption value is shown here as an example for the wavelength set for measuring channel 1:

Int

zero

Abs

log

Int

akt

where:

Int

The intensity measured when

zero

recording the zero spectrum at the wavelength set for measuring channel 1.

Int

The actual intensity measured at

akt

the wavelength set for measuring channel 1.

If you are working with a reference channel (can be activated on the subtab

Configuration) the

formula is as follows:

844 UV/VIS Compact IC / Gebrauchsanweisung 8.844.1051

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Int

refzero

loglog

−

Int

refakt

Abs

Int

zero

Int

akt

where:

Int

The intensity measured when

refzero

recording the zero spectrum at the wavelength set for the reference channel.

Int

The actual intensity measured at

refakt

the wavelength set for the reference channel.

Intensity The intensity (y-axis) is given as a function of

the wavelength (x-axis).

Zero A click on Zero shows the last zero spectrum to

have been recorded (a zero spectrum is

recorded by clicking on the the subtab

Manual/Detector of the 844 control

button on

window).

The zero spectrum is a reference spectrum. It should be recorded at a time at which there is no sample in the measuring cell. It is used for calculating the absorption spectrum (see above formulas).

Wavelength, nm Sets the shown x-axis range

Entry range: 190 ... 900 nm , (standard settings 190 nm and 900 nm, than

Lower limit).

Spectrum Sets the shown y-axis range

Standard settings:

Spline

Activates curve smoothing.

<Apply> Send values to the 844 UV/VIS Compact IC. <Save as> Opens the dialog for entering the path and file

Upper limit must be higher

0 ... 100.

name. Saves the last recorded spectrum in the selected .cvs-file. Format: 2 lines of floating numbers (first line: wavelength, second line: absorption or intensity).

<Copy> Copies plot into clipboard. <Close> Closes window.

If a right-hand mouse click is made in the spectrum window the wavelength

Current spec. value will be shown.

Current wavelength and the corresponding absorption value

4.1 Practical notes on ion chromatography

4 Notes - Maintenance

- Faults

4.1 Practical notes on ion chromatography

4.1.1 Separating columns

Separation efficiency

The attainable quality of analyses with the 844 UV/VIS Compact IC depends to a large extent on the separation efficiency of the column used. When purchasing an IC column you should ensure that the separation efficiency suffices for the analysis problems at hand. Ascertain the characteristic data of the IC column on the standard chromatogram enclosed with the column such as capacity factors, selectivity, plate number and resolution and check these data with your own measurements. If any difficulties arise, you should always first check the quality of the column by recording a standard chromatogram.

Detailed information about the separating columns available from Metrohm can be found in the data sheet accompanying your separating column, in the Metrohm IC Column Catalog, which is available from your local Metrohm agency, or on the Internet under

rohm.com in the ion chromatography product sector. Information about

special IC applications can be found in the relevant "Application Bulletins" or "Application Notes"; these are available on the Internet under requested free of charge from your local Metrohm agency.

Protection

To protect the column against foreign particles which could have an adverse influence on the separation efficiency, we advise you to subject both the eluents and all samples to microfiltration (0.45 μm filter) and to siphon the eluent through the 6.2821.090 Aspirating Filter.

In order to avoid contamination by particles it is advisable to mount an in-line filter between the pump and injection valve. In the 844 UV/VIS Compact IC a 6.2821.120 PEEK filter unit / 6.2620.180 Filter unit Steel is already mounted (see Section

The use of readily interchangeable precolumns serves to protect the actual separating columns and increase their service life appreciably. The precolumn that is suitable for your separating column can be found in the Metrohm IC Column Catalog which is available from your local Metrohm agency, the data sheet accompanying your separating column, the product information about separating columns that can be found under or let your agency advise you directly.

http://www.metrohm.com in the applications sector, or can be

2.3.5 / 2.3.6).

http://www.metrohm.com, ion chromatography products,

http://www.met-

844 UV/VIS Compact IC / Gebrauchsanweisung 8.844.1051

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Storage

Always store the separating columns sealed when not in use and filled in accordance with the manufacturer’s specifications.

Regeneration

If the separation properties of the column have deteriorated, it can be regenerated in accordance with the column manufacturer’s specifications. With the separating columns available from Metrohm, the instructions for regeneration can be found on the leaflet enclosed with every column.

In the case of separating columns with carrier material based on silica,

…

only solutions with pH 2

otherwise the columns could be damaged.

7 may be used for regeneration,

4.1.2 High-pressure pump

Pulsation dampener

The MF 6.2620.150 Pulsation dampener belongs to the standard accessories of the PEEK versions of the 844 UV/VIS Compact IC; its installation is described in Section

2.6.2. It is used to reduce interfering

pulsation in highly sensitive measurements and also protects the column material against pressure shocks caused by the injection.

The two steel versions 2.844.0030 and 2.844.0130 are operated without pulsation dampener.

Maintenance

To protect the pump against foreign particles we advise you to subject the eluent to microfiltration (0.45 μm filter) and siphon the eluent through the 6.2821.090 Aspirating filter.

In many cases an unstable baseline (pulsation, flow fluctuations) can be traced to contaminated valves or faulty, leaky piston seals.

Contaminated valves are cleaned by rinsing with water, RBS solution or acetone (see Section

4.2.4). When the cleaned valves are reinstalled

you must ensure that the flow direction is correct.

The replacement of piston seals is described in Section

4.2.4.

It is essential to make sure that no precipitation can occur (see also

Section

4.1.3). This could lead to dirty valves, pressure increases and,

in extreme cases, to scratched pistons.

4.1.3 Eluents

Treatment

For the preparation of the eluents only chemicals of a purity degree of at least "p.a." should be used. Use eluents that are recommended for spectroscopic detection. For diluting please use only high purity water.

4.1 Practical notes on ion chromatography

Fresh eluents should always be microfiltered (0.45 μm filter) and degassed (with N

with low buffering capacity one should preferably use a CO (see Section

2.6.3).

, He or vacuum). For alkaline eluents and eluents

absorber

The supply vessel containing the eluent must be closed as tightly as possible to avoid excessive evaporation. This is primarily important with eluents containing organic solvents (e.g. acetone), the evaporation of which can lead to drifts in the long term. If work is performed in a very sensitive range, even if one drop of condensate falls back in the eluent this can cause a noticeable change in the background conductivity.

Eluent change

When changing the eluent you must make sure that no precipitation can occur. This means that solutions used in sequence must be miscible. If the system needs to be rinsed with organic solvents then it may be necessary to use several solvents with increasing or decreasing lipophilicity (e.g. water ↔ acetone ↔ chloroform).

4.1.4 Peristaltic pump

The 6.1826.110 Pump tubing used in the peristaltic pump is a consumable with a limited working life. This is why you should replace the tubing at regular intervals; when in continuous use this should be approx. every 4 weeks (see Section

The working life of the pump tubing depends to a great extent on the contact pressure, so make sure that this is set correctly according to the instructions given in Section switched off for a longer time, lift up tubing cartridge loosening snap-action lever set optimal contact pressure is retained).

4.1.5 Connections

All connections between injection valve, column and detector must be as short as possible, have a low dead volume and be absolutely tight. The PEEK capillary after the detector block must be free from constriction (the measuring cell is tested to 5 MPa = 50 bar back pressure).

4.2.5).

2.10.2 and, if the pump is to be

96 by fully

98 on the right-hand side (in this way the

The 6.1826.110 Pump tubing is made from PVC and must therefore not be used for rinsing with solutions containing organic solvents. In this case you must use different pump tubing material, or use a different pump for rinsing.

With the PEEK versions 2.844.0010, 2.844.0020, 2.844.0110 and

2.844.0120 only PEEK capillaries are used in the high pressure area.

Use PEEK capillaries with 0.25 mm i.d. for the capillary connection between injection valve

46 and UV/VIS detector 43.

With the Steel versions 2.844.0030 and 2.844.0130 only Steel capillaries are used in the high pressure area.

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4.2 Maintenance and servicing

4.2.1 General information

Care

The 844 UV/VIS Compact IC requires proper care and attention. Excessive contamination of the instrument could possibly lead to malfunctions and a shorter service life of the inherently rugged mechanical and electronic parts.

Spilled chemicals and solvents should be wiped up immediately. It is especially important to protect the plug connections at the rear of the instrument (particular the mains plug) against contamination.

Although constructional measures have been designed to virtually eliminate such a situation, should corrosive media penetrate the interior of the instruments the mains plug of the 844 UV/VIS Compact IC must be immediately disconnected to prevent extensive damage to the instrument electronics. Inform Metrohm service if your instrument(s) have been damaged in such a way.

The instrument must not be opened by untrained personnel. Please comply with the safety notes in Section

Maintenance by Metrohm service

Maintenance of the 844 UV/VIS Compact IC is best done as part of an annual service performed by specialists from the Metrohm company. If work is frequently performed with caustic and corrosive chemicals, it may be necessary to shorten the interval between servicing.

The Metrohm service department is always willing to offer expert advice on the maintenance and servicing of all Metrohm instruments.

4.2.2 Shutdown

If the 844 UV/VIS Compact IC is shut down for a considerable length of time, the entire IC system (without salt with methanol/water (1:4) to avoid crystallization of eluent salts with the corresponding subsequent damage.

The connections to the column must be removed for rinsing; the two inlet and outlet capillaries are connected directly with a coupling.

Before taking it back into operation, rinse the system with eluent (before the connection of the separation column).

1.4.1.

column) must be rinsed free from

4.2.3 Changing separating columns

It is recommended that the precolumn is also changed each time you change the separation column). In principle the precolumn requires changing more frequently then the separating column.

Identical separation system

4.2 Maintenance and servicing

If you wish to replace an IC separating column by a column of the same type, proceed as follows:

1 Remove old column

• Switch off high-pressure pump and wait for pressure to drop.

• With column heating: screw off knurled screws 116, remove

117.

cover

• Screw off the column connection capillaries (both sides) from the column or precolumn.

2 Connect new column to injection valve

• Remove end caps from column 113.

• Screw inlet end of column

column inlet capillary

Section

2.8.1).

113 (observe flow direction) onto

47/110 or onto the precolumn (see

3 Rinse column

• Place beaker beneath the column outlet.

• Switch on high-pressure pump and rinse column with eluent

for approx. 10 min, then switch off pump.

4 Connect column to detector block

• Screw outlet end of column 113 onto column outlet capillary (depends on Version: (2.844.0020/2.844.0120) or

122(2.844.0010/2.844.0110), 123

124 (2.844.0030/2.844.0130)).

Changing the separation system

If you wish to replace an IC separating column by a column of a different type, proceed as follows:

1 Remove old column

• Switch off high-pressure pump and wait for pressure to drop.

• With column heating: screw off knurled screws 116, remove

117.

cover

• Screw off the column connection capillaries (both sides) from the column or precolumn.

2 Rinse with eluent

• Place a beaker beneath column inlet capillary 47/110.

• If the new eluent is not miscible with the previous eluent then

you must rinse the IC system for approx. 15 min with a solvent in which both the eluents are miscible.

• Rinse the IC system for approx. 15 min with the eluent required for the column that is later to be used (flow rate 1 mL/min).

3 Connect new column to injection valve

• Remove end caps from column 113.

• Screw inlet end of column

column inlet capillary

Section

844 UV/VIS Compact IC / Gebrauchsanweisung 8.844.1051

2.8.1).

113 (observe flow direction) onto

47/110 or onto the precolumn (see

Table of contents

4 Rinse column

• Place beaker beneath the column outlet.

• Set flow rate for new separating column.

• Switch on high-pressure pump and rinse column with eluent

for approx. 10 min, then switch off pump.

5 Connect column to detector block

• Screw outlet end of column 113 onto column outlet capillary

(depends on Version: (2.844.0020/2.844.0120) or

122(2.844.0010/2.844.0110), 123

124 (2.844.0030/2.844.0130)).

4.2.4 Maintenance work at the pump head

In many cases, an unstable baseline (pulsation, flow fluctuations) can be traced to contaminated valves or faulty, leaky piston seals at the high-pressure pump. For cleaning contaminated valves and/or replacement of wear parts such as pistons, piston seals and valves, proceed as follows:

1 Detach pump head

• Switch off pump drive of the IC Pump.

• Disconnect aspirating tubing

at the pump head

27/54.

• Unscrew connection capillary

82 from aspirating capillary 30

24/52 from the pump head

27/54.

• Remove the pump head

27/54 by slackening the 4 securing

screws on the front of the pump head with the aid of the Allen key 6.2621.030 from the pump housing. The main piston is located at the left (when viewed from the front) and the auxiliary piston is located at the right.

2 Disassemble pump head

• Strip down pump head 27/54. Main and auxiliary pistons are

identical with the following exceptions:

- The spring 136 of the auxiliary piston (right piston) is more

powerful (longer) than that of the main piston (left piston).

- Inlet and outlet valve are not present in the secondary cy-

linder.

To prevent the piston cartridge

137

, the screw

134

suddenly jumping out of the piston

133

must be undone very carefully by hand.

3 Cleaning/replacement of piston 134

• Pistons contaminated by abrasive particles or deposits are cleaned with scouring powder and rinsed free of any particles with dist. water.

• Relatively badly contaminated or scratched pistons must be replaced (spare part: 6.2824.070 Zircon piston).

4.2 Maintenance and servicing

4 Replacement of piston seal 140

• To remove damaged piston seals 140 the special tool 144 is

used. This is screwed into the seal pulled out (see Figure 27 A).

144

When the special tool the latter is completely destroyed!

• To install a new piston seal

• First the new seal is inserted firmly in the recess of tool 145

by hand (see Figure 27 B). The seal spring must be located on the outside.

• The tool pump head recess with the aid of tool

145 together with the seal is then inserted in the

27/54 and the seal pressed into the pump head

is screwed into the piston seal

140 the special tool 145 is used.

144 (see Figure 27 C).

140, which can then be

140

133 134

Figure 26: Components of the pump head

135

136

27/54

137

138

139

143

142

143

140

143

844 UV/VIS Compact IC / Gebrauchsanweisung 8.844.1051

Table of contents

144

Figure 27: Replacement of the piston seal

27/

Pump head 6.2824.040/6.2824.100

Screw (3.709.1100) for piston

133

cartridge

137.

145

27/54

140

145

144

140

Piston guide sleeve (4.709.4380)

138

Piston guide sleeve (4.709.4370)

139

Piston seal (6.2741.020)

140

Zirconium piston (6.2824.070) with

134

piston shaft

Spring retainer

135

Spring (6.2824.050) for main piston

136

or Spring (6.2824.060) for auxiliary piston

Piston cartridge (4.709.0760)

137

The seal surface in the pump head (avoid contact with tool)!

5 Cleaning/replacement of inlet valve 141 and outlet

valve 142

Inlet valve 6.2824.020/6.2824.090

141

Outlet valve 6.2824.010/6.2824.080

142

Screw holder for valve

143

Special tool (6.2617.010) to remove

144

the piston seal

Special tool (6.2617.010) to install

145

the piston seal

27/54

• Contaminated or blocked valves are cleaned by rinsing with dist. water, RBS solution or acetone. The rinsing effect can be reinforced by brief treatment in an ultrasonic bath (max. 20 s; if longer the sapphire sphere of the valve can be damaged).

• If this does not have the desired effect, the valves can be disassembled as shown in Figure 28. The valve components are pushed out with the aid of a syringe needle inserted

140

144

must not be damaged

4.2 Maintenance and servicing

through the upper opening in the valve housing. The individual components are rinsed with dist. water and/or acetone, and the sapphire sphere cleaned with a paper towel. The valve is then reassembled in accordance with Figure 28. The components of the inlet and outlet valves are identical, they are distinguished only by the positioning of the ceramic holder

• Valves that fail to function faultlessly after such cleaning must be replaced.

• In the reinstallation of the inlet valve

142 on no account must the two outwardly identical valves be

interchanged. To determine which valve is which, note that the liquid flows through the pump head from the bottom up. The flow direction of the valves can be checked simply by blowing through the clean valve. Both valves are installed with the black face in the direction of the pump head (see Figure

28).

If by mistake an inlet valve

142

, an extreme pressure buildup occurs within the working cylinder,

which is not detected by the pressure transducer and will destroy the

140

piston seal

151 (see Figure 28).

141

is installed instead of the outlet valve

141 or the outlet valve

6 Mounting the pump head

• Reassemble the components of the pump head 27/54 as

shown in Figure 28. Tighten the screw screw in piston cartridge reached and then use a wrench to turn it through a further 30°. Firmly tighten the two valve screw holders wrench.

• Reattach pump head 4 fixing screws. Firmly tighten them with the 6.2621.030 Allen key.

To ensure that the pump head is not positioned wrongly, the holes at the rear for the clamping bolts have different depths, i.e. 1 clamping bolt is longer than the rest. The deepest hole must naturally accommodate the longest bolt. If this is not the case, the pump will not function properly.

• Screw connection capillary

• Connect aspirating tubing

pump head

27/54.

27/54 to the pump with the help of the

133 by hand. First

137 manually until the stop is

143 with a

30 to pump head 27/54.

82 to aspirating capillary 30 at the

844 UV/VIS Compact IC / Gebrauchsanweisung 8.844.1051

Table of contents

146

147

148

149

150

151

152

141

Inlet valve

142

Outlet valve

Valve housing

146

Sealing ring (black)

147

Sleeve

148

146

Sapphire sleeve

149

The bright side must point towards the

147

sapphire sphere.

Sapphire sphere

150

148

Ceramic holder for sapphire

151

sphere

151

The large recess must point in the direction of the sapphire sphere

150

Seal

149

152

The larger opening must point outwards

152

141

Figure 28: Components of inlet valve

and outlet valve

4.2.5 Replacing the pump tubing

The pump tubings used by the peristaltic pump are consumable material with a limited lifetime and should be exchanged at regular intervals (approx. every 4 weeks under continuous use).

The working life of pump tubing depends to a considerable extent on the contact pressure. This is why the contact pressure must be correctly set as described in Section switched off for a lengthy period of time the tubing cartridges be raised completely by loosening the snap-action lever hand side (the set contact pressure remains unchanged).

As the pump is always operated on the same side the 6.1826.110 Pump tubings supplied can be used on both sides. To exchange a pump tubing proceed as follows:

1 Remove old pump tubing

• Press contact pressure lever 97 on the tubing cartridge 96

down as far as it will go.

• Release tubing cartridge action lever

• Remove old pump tubing

98 and remove from mounting pin 40.

142

2.10.2. If the pump is to remain

96 should

98 on the right-

96 from 50 by pressing down snap-

94.

4.2 Maintenance and servicing

2 Insert new pump tubing

• Insert the new pump tubing 94 in the tubing cartridge 96 as

shown in Figure 17. The orange-yellow stopper into the corresponding holder on the left-hand side of the tubing cartridge.

• Place the tubing cartridge down on the right-hand side until snap-action lever into position on holding clamp formed in the pump tubing.

3 Set contact pressure

• Switch on peristaltic pump.

• Press contact pressure lever

just starts to be drawn in. Then press contact pressure lever upwards until it clicks once more to obtain optimal contact pressure.

• Switch off peristaltic pump.

96 on mounting pin 40 and press

50. Take care that no kinks are

97 upwards until the solution

95 must click

98 clicks

4.2.6 Replacing the UV lamp

Proceed as follows to replace the UV lamp:

The UV lamp becomes hot when used for a long time! Allow it to cool down before you start to replace it.

Avoid contact with the surface of the lamp! Residues reduce the light transmittance and may also be burned into the glass and cause permanent damage.

If it becomes dirty the lamp surface should be cleaned with alcohol before it is used again.

1 Insert lamp

• Insert UV lamp 153 into the "Opening for UV lamp" 155 at the bottom of lamp cooling housing

2 Screw on fastening ring

• Screw down attachment ring 154. The attachment ring forms part of the 844.

3 Connect cable

• Plug "UV lamp connection cable" 11 into " UV lamp connection"

844 UV/VIS Compact IC / Gebrauchsanweisung 8.844.1051

12 of the 844 UV/VIS Compact IC.

Table of contents

153

154

Figure 29: UV lamp (deuterium)

155

Figure 30: Lamp connections (at the back of the 844 UV/VIS Compact

IC)

9 Lamp cooling housing

11 UV lamp connection cable

UV lamp

153

UV lamp attachment ring

154

Replacing the VIS lamp (halogen) is described on the 8.108.1073 leaflet accompanying the VIS lamp.

Opening for UV lamp

155

Opening for VIS lamp

156

Metrohm 844UV-VIS User Manual

Specifications and Main Features

Frequently Asked Questions

User Manual

1.2 Parts and controls

1.2.2 Rear panel

1.2.3 Interior PEEK versions

1.2.4 Interior Steel versions

1.3 Information on the Instructions for Use

1.3.1 Organization

1.3.2 Notation and pictograms

1.4 Safety notes

1.4.2 General precautionary rules

1.4.3 Recycling and disposal

2 Installation

2.1 Overview

2.1.2 Connections in the 844 UV/VIS Compact IC

2.2 Setting up the instrument

2.3 Attaching the accessories

2.3.1 Connecting the syringe and aspirating tubing

2.3.2 Connecting the drainage tubing for the inner compartment

2.3.3 Connecting PEEK capillaries

2.3.5 Filter unit PEEK

2.3.6 Filter unit Steel

2.4.1 Setting the mains voltage

2.4.3 Mains cable and mains connection

2.4.4 On/off switching of the instrument

2.5.1 Connecting cable

2.5.4 Create a system

2.6.1 Removing the transport security screws

2.6.2 Installing the pulsation dampener

2.6.3 Connecting the eluent bottle

2.6.4 Deaerating the pump and rinsing the pulsation dampener

2.7 Post column reactor

2.7.1 Preparing the peristaltic pump

2.7.2 Installation of the post column reactor

2.7.3 Post column reactor tubing connections

2.7.4 Reagent bottle connection

2.8.3 Connecting the separating column (installation without column heating)

2.9 Detector

2.9.1 Installing the flow-through cell

2.9.2 Connect the lamps

2.9.3 Flow-through cell tubing connections

2.10.1 Putting into operation without post column reactor

2.11 Connection of external devices

2.11.1 Connection of the 838 Advanced Sample Processor

3.1 «IC Net» - Terms

3 Operation

3.2 Measuring operation

3.2.1 Opening a system

3.2.2 Defining measuring channels

3.2.3 Connect a system

3.2.4 Instrument icon

3.2.5 Hardware start/stop and baseline recording

3.2.6 Determination start/stop

3.3 Settings

3.3.1 Instrument control for connected system

3.3.3 Spectrum window

4.1 Practical notes on ion chromatography

4.2.3 Changing separating columns

4.2.4 Maintenance work at the pump head

4.2.5 Replacing the pump tubing

4.2.6 Replacing the UV lamp