Metrohm 817 User Manual

817 Bioscan
Bioscan817
Bioscan
CH-9101 Herisau/Switzerland E-Mail info@metrohm.com Internet www.metrohm.com
Instructions for Use
8.817.1003
CH-9101 Herisau/Switzerland E-Mail info@metrohm.com Internet www.metrohm.com
817 Bioscan
Instructions for Use
8.817.1003 09.2001 / up
Contents

Contents

1 Introduction............................................................................................ 1
1.1 Instrument description............................................................................. 1
1.2 Parts and controls .................................................................................... 2
1.3 Information about the Instructions for Use .......................................... 8
1.3.1 Organization.................................................................................. 8
1.3.2 Notation and pictograms.............................................................. 9
1.4 Safety notes ............................................................................................. 10
1.4.1 Electrical safety........................................................................... 10
1.4.2 General precautionary rules ....................................................... 10
2 Installation........................................................................................... 11
2.1 Setting up the instruments.................................................................... 11
2.1.1 Packaging ................................................................................... 11
2.1.2 Check.......................................................................................... 11
2.1.3 Location ...................................................................................... 12
2.1.4 Arrangement of the instruments................................................. 12
2.2 Mains connection ................................................................................... 12
2.2.1 Setting the mains voltage ........................................................... 12
2.2.2 Fuses .......................................................................................... 13
2.2.3 Mains cable and mains connection ........................................... 14
2.2.4 On/Off switching ......................................................................... 14
2.3 Capillary connections ............................................................................ 15
2.3.1 Connection of the 6.5324.000 Bottle Rack (option)................... 15
2.3.2 Connection of the pulsation absorber........................................ 15
2.3.3 Connection of the injection valve ............................................... 16
2.3.4 Mounting the column.................................................................. 16
2.3.5 Connection of the flow cell ......................................................... 17
2.3.6 Connecting the waste tubing...................................................... 18
2.3.7 Rinsing the tubing....................................................................... 19
2.3.8 Rinsing the column ..................................................................... 19
2.4 System for sugar analysis – MIC 8 ...................................................... 20
2.4.1 Electrical connections................................................................. 20
2.4.2 Settings in «IC Net 2.1» ............................................................. 21
2.4.3 Connecting a sample changer ................................................... 22
2.5 System for the analysis of anions and sugars – MIC 9.................... 24
2.5.1 Electrical connections................................................................. 24
2.5.2 Capillary connections ................................................................. 25
2.5.3 Configuration in «IC Net 2.1» ..................................................... 27
2.6 Preparing the 817 Bioscan for the analysis ....................................... 32
2.6.1 System switch-on........................................................................ 32
2.6.2 Start pump .................................................................................. 32
2.6.3 Set operating mode.................................................................... 33
817 Bioscan
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Contents
3 Operation............................................................................................... 35
3.1 Handling the 817 Bioscan ..................................................................... 35
3.2 Operation using «IC Net 2.1» ................................................................ 36
3.2.1 817 Bioscan icon.........................................................................36
3.2.2 817 Bioscan window ...................................................................37
4 Basic principles............................................................................. 47
4.1 Introduction ............................................................................................. 47
4.2 Measuring conditions ............................................................................ 48
4.3 Pulsed amperometric detection........................................................... 49
4.3.1 Optimization of the PAD parameters ..........................................49
4.4 Optimization of the measuring potential ............................................ 51
5 Notes – Maintenance – Faults....................................... 55
5.1 Practical notes on ion chromatography ............................................. 55
5.1.1 Separating columns ....................................................................55
5.1.2 High-pressure pump ...................................................................56
5.1.3 Eluents .........................................................................................57
5.1.4 Connections ................................................................................57
5.2 Maintenance and servicing................................................................... 58
5.2.1 General information .....................................................................58
5.2.2 Shutdown.....................................................................................58
5.2.3 Cleaning the working electrode ..................................................59
5.2.4 Changing separating columns....................................................60
5.3 Faults and malfunctions ........................................................................ 61
5.3.1 Malfunctions and their rectification .............................................61
5.4 Instrument test with the dummy cell ................................................... 63
5.5 Validation / GLP ...................................................................................... 64
6 Appendix................................................................................................. 65
6.1 Technical data......................................................................................... 65
6.2 Standard equipment............................................................................... 69
6.3 Warranty and conformity....................................................................... 71
6.3.1 Warranty.......................................................................................71
6.3.2 EU declaration of conformity.......................................................72
6.3.3 Certificate of conformity and system validation ..........................73
6.4 Index ......................................................................................................... 75
II
817 Bioscan
Contents
List of illustrations
Fig. 1: Front of the 817 Bioscan................................................................................... 3
Fig. 2
: Rear of the 817 Bioscan.................................................................................... 4
Fig. 3
: Interior of the 817 Bioscan (with permanently attached accessories) .. 6
Fig. 4
: Setting the mains voltage ............................................................................... 13
Fig. 5
: Connections at the injection valve of the 2.812.0010 Valve Unit ......... 16
Fig. 6
: Connections at flowcell ............................................................................... 17
Fig. 7
: Connecting up a simple modular IC system
with the 817 Bioscan – MIC 8
Fig. 8
: Connecting up a simple MIC 8 system
including a sample changer
Fig. 9
: Connections with a 817 Bioscan as second detector
with a modular IC system – MIC 9
..................................................................... 20
....................................................................... 22
............................................................. 24
Fig. 10
: Connections of injection valves A and B in the IC Separation
Center (2.733.0120)
Fig. 11
: Potentials applied during pulsed amperometric detection (PAD). ...... 49
Fig. 12
: Example of a hydrodynamic voltammogram of a
..................................................................................... 26
substance (A) with additional presentation of the measured values for the pure eluent (B)
Fig. 13
: Example of a scan of a substance (A) with additional
presentation of the scan of the pure eluent (B)
.................................................. 51
...................................... 52
817 Bioscan
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Contents
IV
817 Bioscan
1.1 Instrument description

1 Introduction

1.1 Instrument description

The 2.817.0010 Bioscan is a PC-controlled measuring instrument for the sensitive analysis of carbohydrates by ion chromatography using pulsed amperometric detection. The compact housing of the 817 Bio­scan contains several IC system components:
Detector – flow-through cell with three-electrode arrangement for
amperometric detection in the Pulse, DC and Scan modes.
Column compartment – the perfect insulation of the housing cre-
ates not only stable thermal conditions for the separating columns, but also shields the system from electromagnetic interference; in addition to the column it also contains the detection cell, pulsation absorber and preheating capillary.
Oven – amperometric determinations require extremely stable
thermal conditions. The built-in column compartment oven ensures that all important components can be set exactly to a temperature from 10°C above room temperature to 60 °C with a stability of
0.1°C.
All components that come into contact with the eluent and the
sample, except the electrodes, are metal-free.
Signal converter – the 817 Bioscan contains its own analog/ digi-
tal converter for the detector signal. This means that complete con­trol of the instrument is possible from a PC via an RS232 interface.
Together with the 709 IC Pump and the 812 Valve Unit, the 817 Bio-
scan forms a complete IC system for carbohydrate analysis. Opera­tion is via a PC connected to the RS232 interface and uses the in-
cluded «IC Net 2.1» control and evaluation program. This software fulfills all the demands which are placed today on a modern integration software: 1-point or multi-point calibration, internal or external standard, selectable algorithms for non-linear calibration, numerous Integration modes with selectable parameters and integration events, various peak recognition methods, peak editor, free scaling, superimposition of sev­eral chromatograms, post-treatment of chromatograms, high-perform­ance GLP-conform report generator with output interfaces for monitor, printer and external databases.
817 Bioscan
1
1 Introduction
817 Bioscan
2

1.2 Parts and controls

1.2 Parts and controls
Bioscan817
Bioscan
1 2 3
: Front of the 817 Bioscan
Fig. 1
Door to interior 3 Feed through for tubing
1
e.g. connection of injection valve and pre­heating capillary or connection to waste
2 Feed through for tubing
e.g. connection of 709 IC Pump and pulsation absorber
817 Bioscan
3
1 Introduction
4
4
4
4
5
6
4
4
7
8
18
17
9
16
4
10
11 14
12 13 15
Fig. 2
: Rear of the 817 Bioscan
4
817 Bioscan
4
1.2 Parts and controls
Mounting screw
4
for fastening the rear panels 5 / 6
12 Lower connections for remote lines
(not used with IC Net)
Detachable rear panel
5
access to top part of the inner com­partment
6 Detachable rear panel
access to bottom part of the inner compartment
7 Analog signal (REC.)
AD/DA-converted signal (not used with IC Net; see chapter 6.1 for details)
8 Analog signal (Int.)
Original signal (not used with IC Net; see chapter 6.1 for details)
9 Manual valve
(not used with IC Net)
10 Model plate
with technical data serial number
13 Outlet for spilled liquid
for discharge of spilled liquid from the inner compartment
14 RS232 interface
connection of the PC; see chapter 6.1 for details
15 Upper connections for remote lines
Aux 1, Aux 2 as well as 1 and 2 are
only used with IC Net
16 Fuse holder
changing the fuses, see section 2.2.1
17 Mains connection plug
mains connection, see section 2.2
18 Mains switch
to switch instrument on and off: I = ON 0 = OFF
11 Electric valve
(not used with IC Net)
817 Bioscan
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1 Introduction
19 20
21
34
22 23
24
25
26
27
33
1
Metrosep
Carb 1
32
2
29 31
28
: Interior of the 817 Bioscan
Fig. 3
30
(with permanently attached accessories)
3
817 Bioscan
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1.2 Parts and controls
Electrode cable (red)
19
connection for working electrode
27 Connection for elektrode cable
connection '1'
Electrode cable (blue)
20
connection for auxiliary electrode
28 Connection capillary
connection 709 IC Pump – pulsation absorber
21 Column connection capillary
PEEK capillary
29 Connection capillary
connection pulsation absorber – injection valve
22 Measuring cell holder 30 Pulsation absorber
6.2620.150
23 Au - Flow cell
6.1254.010
24 Electrode cable (black)
connection for reference electrode
25 IC column
e.g. Metrosep Carb 1 (6.1013.000)
31 Preheating capillary
6.1836.010, length: 3 m
32 Oven
33 Oven heating fan
for carbohydrate analysis
26 Column holder
34 Connection capillary
connection flow cell – waste
817 Bioscan
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1 Introduction

1.3 Information about the Instructions for Use

Please read through these Instructions for Use carefully before you put the 817 Bioscan 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 instruments.

1.3.1 Organization

These Instructions for Use 8.817.1003 for the 817 Bioscan provide a comprehensive overview of the startup procedure, operation, fault recti­fication and technical specifications of these instruments. The Instruc­tions for Use are organized as follows:
Section 1 Introduction
General description of instruments, parts and controls and safety notes
Section 2 Installation
Setting up, mains connection, attachment of accesso­ries, connection to IC system
Section 3 Operation
Detailed description of the operation
Section 4 Basics
Information about the pulsed amperometric detection
Section 5 Notes – Maintenance – Faults
Notes on ion chromatography, maintenance, fault rectifi­cation, diagnostic tests, validation
Section 6 Appendix
Technical data, standard equipment, options, warranty, declarations of conformity, index
To find the required information on the instrument, you will find it an ad­vantage to use either the Table of contents or the Index at the back.
As a supplement to the Instructions for Use, the 8.732.2003 Metrohm Monograph "Ion chromatography" is also supplied. This provides an introduction to the theoretical fundamentals and general information on separating columns and sample pretreatment.
The 8.792.5003 Metrohm Monograph "Practical Ion Chromato- graphy" is a practical textbook, which provides an illustrative introduc­tion to the basic principles of ion chromatography and also describes 22 experiments covering the whole world of ion chromatography.
IC Application Notes for different applications of Metrohm IC systems are also supplied.
8
817 Bioscan
1.3 Information about the Instructions for Use

1.3.2 Notation and pictograms

The following notations and pictograms (symbols) are used in these In­structions for Use:
<PARAM> Key
'Range' Parameter or entry value
35 Part or control of 817
22 Part or control of 709
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.
817 Bioscan
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1 Introduction

1.4 Safety notes

1.4.1 Electrical safety

While electrical safety in the handling of the 817 Bioscan is assured in the context of the specifications EN61010-1 / IEC61010-1, the following points 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 instruc-
tions in section 2.4.
Opening the 817 Bioscan
If the 817 Bioscan is connected to the power supply, the instrument must not be opened (apart from the front door) nor must parts be removed from it, otherwise there is a danger of coming into contact with components which are live. Hence, always disconnect the instrument from all voltage sources before you open it and ensure that the mains cable is disconnected from mains connection 17 !
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 817 Bioscan, you should earth yourself and any tools you are using by touching an earthed 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.
Never block drain opening for spilled liquids
On the bottom of the interior directly below the front door there is a drain opening 1. Spilled liquids can flow directly to the outlet 13 on the back. Due to safety consideration, take care that these openings may never be blocked.
10
817 Bioscan
2.1 Setting up the instrument

2 Installation

The 817 Bioscan is an electrochemical detector and can be included in a modular IC system in two different ways:
1) The 817 Bioscan as the only detector in an IC system.
Apart from the 709 IC Pump, you also require an 812 Valve Unit with one injection valve. In this MIC-8 modular IC system the 817 Bioscan is intended for the analysis of sugars only.
2) The 817 Bioscan is included in an IC system as the second detector. An example of this is given in Section 2.5 where an IC system (MIC-9) is described for the simultaneous determination of sugars and anions with chemical suppression.
These modular IC system configurations (MIC-1, MIC-2, etc.) are pos­sible instrument combinations that have been properly tested. Under
www.metrohm.com
updated.
you will find further examples; these are continually
Following the general information about the installation of the instruments, Sections 2.4 and 2.5 describe the two configurations mentioned above including their control by the «IC Net 2.1» software.

2.1 Setting up the instrument

2.1.1 Packaging

The 817 Bioscan is supplied together with the separately packed accessories in special packaging containing shock-absorbing foam linings designed to provide excellent protection. The actual instruments are packed in an evacuated polyethylene bag to prevent the ingress of dust. Please store all this special packaging as only it can assure transport of the instruments free from damage.

2.1.2 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 6.2). In the case of transport damage, see instructions in section 6.3.1 "Warranty".
817 Bioscan
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2 Installation

2.1.3 Location

Position the instruments in the laboratory at a location convenient for operation, free from vibrations and protected against a corrosive at­mosphere and contamination by chemicals. The same applies to all other components of the IC system.
To avoid disturbing temperature influences on the insulated column compartment, the entire system including pump and eluent reservoir must be protected against direct sunlight.

2.1.4 Arrangement of the instruments

If the 817 Bioscan is used as a single detector (see chapter 2.4), the 709 IC Pump, 812 Valve Unit and 817 Bioscan are best stacked on top of one another in this order.
In a two-channel system (see chapter 2.5), the optimum arrangement (1, 2 or 3 towers) depends on the laboratory space available.
In general, the IC pumps should be set up at the very bottom and the IC detectors at the very top.

2.2 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!

2.2.1 Setting the mains voltage

Before switching on the 817 Bioscan for the first time, check that the mains voltage set on the instrument (see Fig. 4) matches the local mains voltage. If this is not on the instrument as follows:
1 Disconnect mains cable
Disconnect mains cable from mains connection plug 17.
the case, you must reset the mains voltage
2 Remove fuse holder
Using a screwdriver, loosen fuse holder 16 below the mains connection plug and take out completely.
3 Check and change fuse if necessary
Carefully take the fuses installed for the desired mains voltage out of fuse holder and check their specifications:
100120 V 3.15 A (slow-blow) Metrohm No. U.600.0021
220240 V 1.6 A (slow-blow) Metrohm No. U.600.0018
817 Bioscan
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2.2 Mains connection
V
V
4 Insert fuse
Change fuses if necessary and reinsert in fuse holder.
5 Install fuse holder
Depending on the necessary mains voltage, insert fuse holder in the 817 Bioscan so that the corresponding mains voltage range can be read normally and the adjacent white arrow points to the white bar imprinted below the fuse holder (see Fig. 4).

2.2.2 Fuses

18
17
100 – 120
220 – 240
18 Mains switch
17 Mains connec-
tion plug
16
220 - 240 V
100 - 120 V
100 - 120 V
220 - 240 V
16 Fuse holder
Fig. 4
: Setting the mains voltage
Two fuses 3.15 A/slow-blow for 100120 V or 1.6 A/slow-blow for 220240 V are installed in fuse holder 16 of the 817 Bioscan as stan­dard.
Ensure that the instrument is never put into operation with fuses of a different type as this could cause a fire!
817 Bioscan
For checking or changing fuses, proceed as described in section 2.2.1.
13
2 Installation

2.2.3 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 an earthing pin. If a dif­ferent plug has to be fitted, the yellow/green lead (IEC standard) must be connected to protective earth (protection class 1).
Any break in the earthing inside or outside the instrument can make it a hazard!
Mains connection
Plug the mains cable into mains connection plug 17 of the 817 Bioscan (see Fig. 2).

2.2.4 On/off switching of the instruments

The 817 Bioscan is switched on and off using mains switch 18. Do not switch the IC components on before all cable connections have been established.
817 Bioscan
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2.3 Capillary connections

2.3 Capillary connections

The capillary connections described below are necessary for operating the 817 Bioscan in a simple IC system for carbohydrate analysis (MIC-
8). The electronic connections and control by IC Net 2.1 are described in Section 2.4.
Section 2.5 contains the description of a combination of this IC system with an IC system for the determination of anions with chemical sup­pression (MIC-9). The necessary changes to the capillary connections are described there.

2.3.1 Connection of the 6.5324.000 Bottle rack (option)

The optionally available 6.5324.000 Bottle rack for supply vessels can be placed on top of the 817 Bioscan. The tubing connections to the 709 IC Pump are described in the corresponding leaflet.

2.3.2 Connecting the pulsation absorber

To protect the column material from any pressure shocks which the in­jection may cause we recommend the insertion of the 6.2620.150 MF Pulsation absorber between the high-pressure pump and the injec­tion valve. This is done as follows (see Fig. 3):
1 Connect the pulsation absorber
Place pulsation absorber 30 on the floor in the interior of the 817 Bioscan.
2 Connection to pump
Connect the 6.2821.100 PEEK Filter unit described in Section 2.3.5 of the 8.709.1021 ‘Instructions for Use’ to con­nection 23
Lead PEEK capillary 28 or 43 the filter unit outwards through opening 2 of the Bioscan and attach it to one of the 52 connections on the top side of the pulsation absorber.
3 Connection to injection valve
Connect PEEK capillary 29 to the second connection 30 of the pulsation absorber, lead it out through 2 of the Bioscan and connection it to the injection valve on the 812 Valve Unit (connection 17).
The pulsation absorber is filled with isopropanol and must be rinsed with eluent before a separating column is connected (see Section
2.3.7).
of the 709 Pump by using PEEK capillary 22.
from connection piece 47 of
817 Bioscan
The 6.2620.150 Pulsation absorber can be operated in both direc­tions.
15
2 Installation

2.3.3 Connection of the injection valve

Connect all capillaries to the injection valve according to the following description:
46 45
45
36
21
4447
Fig. 5
: Connections at the injection valve of 2.812.0010 valve unit
Connection for syringe tubing
42
PTFE tubing with coupling (6.2744.120) and syringe (6.2816.020, without needle)
43
Connection for aspirating tubing
PTFE tubing for aspirating sample
44 Connection for sample loop
20 µL PEEK sample loop (6.1825.210)

2.3.4 Mounting the column

The IC separating column (e.g. Metrosep Carb 1, 6.1013.000) is first mounted in the 817 Bioscan as follows (see Fig. 3):
42 43
45 Eluent outlet
Connection to preheating capillary 31 (PEEK, 6.1836.010)
46 Eluent inlet
PEEK capillary connection 29 to pulsation absorber
47 Connection for sample loop
20 µL PEEK sample loop (6.1825.210)
1 Connect column to the preheating capillary
Remove the caps from column 25.
Screw eluent outlet of preheating capillary 31 on to the inlet
end of the column (observe flow direction) .
2 Connect column to flow-through measuring cell
Screw outlet end of column 25 on to eluent inlet 41 of the
flow-through cell using the 6.2744.130 KELF pressure screw.
3 Fix column
Fix the column in column holder 26.
817 Bioscan
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2.3 Capillary connections

2.3.5 Connection of the flowcell

The Flowcell (6.1254.010) is a part of the standard equipment of the 817 Bioscan. It is already mounted and ready to use.
37
36
38
35
39
41
40
: Connections at flowcell
Fig. 6
Check marks
35
For correct orientation of the top and bottom part of the flow-cell
36
Mounting screws (4x)
37 Outlet for eluent
Connection of PEEK capillary by
6.2744.130 KELF pressure screw . PEEK pressure screws may damage the threads of the cell.
38 Working electrode connection
for red electrode cable 19
39 Auxiliary electrode connection
for blue electrode cable 20
40 Reference electrode connection
for black electrode cable 24
41 Inlet for eluent
Connection of PEEK capillary by
6.2744.130 KELF pressure screw. PEEK pressure screws may damage the threads of the cell.
817 Bioscan
1 Before starting up check all screws 36
Use the Allen key provided to loosen all four of the 36 screws by one rotation.
Then slightly tighten the screws again, e.g. by holding the Allen key between the thumb and index finger only.
Finally tighten all four screws by a quarter rotation.
Always tighten opposing screws, i.e. tighten one screw and
then the opposite screw.
Avoid overtightening the screws as this could damage the
6.1254.020 Distance piece!
17
2 Installation
2 Connect the electrode cable
The included 6.2156.000 Cable for connecting the measur-
ing cell is attached to connections 38, 39 and 40 of the measuring cell using the three connectors 19, 20 and 24 (see Fig. 6).
The other end of the cable is inserted into connection '1' of
the 817 Bioscan 817 with connector 27 (see Fig 3).
3 Connect the column
Screw column connection capillary 21 of the column on to eluent inlet 41 of the flow-through measuring cell using the
6.2744.130 Pressure screw.
4 Connect the waste container
In order to ensure an adequate backpressure, screw a PEEK capillary (approx. 1 m) on to eluent outlet 37 of the measuring cell.
Lead the end through opening 3 into a sufficiently large waste container and attach it there.
5 Mount the measuring cell
Attach the flow-through measuring cell to the holder 22 817 Bioscan which is provided for it (see Fig. 3).
Rotate the holder and the cell so that the cell outlet is located as high as possible. In this way it is easier for any air bubbles that may occur to escape from the cell.
Never switch on the flow-through cell when this is (a) not being rinsed through with a conducting eluent at the
time, (b) not completely connected up, or (c) when its outside is moist so that so a short circuit could
occur between the connections of working electrode 38
and auxiliary electrode 39!

2.3.6 Connecting the waste tubing

The 817 Bioscan has an outlet 13 on its rear panel for discharged liquids to which the waste tubing can be attached. Proceed as follows:
1 Connect the waste tubing
Attach matching tubing (e.g. Silicone tubing, optional) into
outlet 13 (see Fig. 2).
2 Lead the waste tubing to a drain
Place the other end of the waste tubing in a drain and attach it there.
817 Bioscan
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2.3 Capillary connections

2.3.7 Rinsing the tubing

The pulsation absorber is supplied permanently mounted and is filled with isopropanol. In order to remove this and any air that may be pre­sent in the capillaries and the measuring cell all the eluent-carrying tub­ing or capillary connections must first be installed; the column and the flow cell must not be connected during the beginning of the process.
Proceed as follows:
1 Deconnect preheating capillary from column
Deconnect the eluent outlet of preheating capillary 31 from the column and fix it at a waste bottle.
2 Set injection valve to “Inject”
Press the <INJECT> key on the 812 Valve unit, which should not yet be connected to the 817 Bioscan. The green LED in the key lights up to show that the injection valve is in the “In­ject” position.
3 Vent 709 IC Pump before start up
Proceed according to Section 2.7 of the ‘Instructions for Use’ of the 709 IC Pump.
4 Rinse with dist. H2O
Immerse the aspiration capillary of the 709 IC Pump in dis­tilled or deionized water.
Switch on the 709 IC Pump, rinse the IC system for approx. 10 min. and switch off the 709 IC Pump.
5 Rinse with eluent
Immerse the aspiration capillary of the 709 IC Pump in the eluent to be used (e.g. 100 mM NaOH).
Switch on the 709 IC Pump, rinse the IC system for approx. 10 min. and switch off the 709 IC Pump.
6 Connect flowcell and rinse with eluent
Connect the preheating capillary 31 to flowcell using column connection capillary 21 and 6.2620.060 Coupling.
Switch on the 709 IC Pump, rinse the IC system for approx. 10 min. with eluent and switch off the 709 IC Pump.
7 Remove the coupling
Remove the 6.2620.060 Coupling between column connec­tion capillary 21 and preheating capillary 31.
Remount the column between column connection capillary 21 and preheating capillary 31 as show in Fig. 3.

2.3.8 Rinsing the column

In order to rinse or precondition the column the connection capillary 21 to flowcell must be unscrewed from the column. Proceed as described in point 3 and 4 in section 5.2.4.
817 Bioscan
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2 Installation

2.4 System for sugar analysis – MIC-8

The MIC-8 system with manual sample injection is described below. Of course, you can also install a Metrohm sample changer. This is de­scribed in Section 2.5 or in the ‘Instructions for Use’ of the sample changer.
In order to connect a sample changer and control it completely you need a further free COM port on your PC. However, we recommend the use of the 762 IC Interface, to which you can then also connect the 709 IC Pump to be controlled by IC Net 2.1.

2.4.1 Electrical connections

The electrical connections of the MIC-8 system, which consists of the 817 Bioscan, the 812 Valve unit and the 709 IC Pump, are made ac­cording to Figure 7:
817
812
709
6.2128.100
6.2125.160
PC
1
AUX 1
AUX 2
123456789
Ground
Fill
2
Inject
: Connecting up a simple modular IC system with the 817
Fig. 7
Bioscan – MIC 8
817 Bioscan
20
2.4 System for sugar analysis – MIC-8

2.4.2 Settings in «IC Net 2.1»

1 System
As in this configuration only the 817 Bioscan is to be directly controlled by IC Net then only this instrument is to be installed as the detector with the help of the system assistant
wizard
.
2 Method
You should first select the standard method supplied for use with your particular column (e.g. for Metrosep Carb 1:
CARB1_250.mtw). You can save any alterations under a different
file name.
3 Data source
Select: Cell( 817 BioScan) as the signal source.
4 Save system
Then save the system (e.g. 817_MIC-8.smt). The following system window should now appear:
New system
5 Connect system and workplace
Under SYSTEM / Control / Connect to workplace connect the new system with the workplace.
At the same time the symbol will appear in the symbol bar.
6 Check measuring cell
If the 817 Bioscan is switched on without the flow-through cell being constantly rinsed by a conducting eluent (e.g. 0.1 M NaOH) then the measuring cell must not be switched on!
You should now check this in the instrument window of the 817 Bioscan (accessed with a double-click with the mouse on in­strument symbol) under
Manual / Cell.
7 Check start mode
Make sure that in this system the 817 Bioscan is standing under
Start with determination under Setup / Start mode.
.
817 Bioscan
21
2 Installation

2.4.3 Connecting a sample changer

If the MIC-8 system described above is to be operated with a Metrohm sample changer then the following connections and settings must be made:
817
1
AUX 1
AUX 2
1 2 3456789
2
CELL OFF
CELL ON
+ 24 V
GROUND
10 11 12
6.2141.140
766/78 8/813
6.2141.140
812
709
6.2128.100
6.2125.160
PC
Ground
Fill
Inject
Fig. 8: Connecting a simple MIC 8 system including a sample
changer
The IC Sample Processor 766, the IC Filtration Sample Processor 788 or the Compact Autosampler 813 can be used as the sample
changer. In this combination of the MIC-8 system the 817 Bioscan is operated as the "Master". The start impulse for the instrument methods to the connected sample changer is transferred via the remote connec­tion (6.2141.140, optional). You can then select any instrument method at the sample changer that is described as being for control with the PC as master. Information about this is given in the corresponding ‘Instruc­tions for Use’.
If a second COM port on the PC or a 762 IC Interface is available for an RS232 connection then the 766 IC Sample Processor or the 788 IC Fil­tration Sample Processor can be connected up via this connection. In this way you can generate your own time programs in IC Net 2.1 for these sample changers. Details are given in the ‘Instructions for Use’ for the particular instrument.
817 Bioscan
22
2.4 System for sugar analysis – MIC-8
Creating the time program
In order to control the 766 IC Sample Processor and the 788 IC Fil­tration Processor the following program is created in the Bioscan:
In this way shortly after the injection valve has been switched to 'Fill' at the 812 Valve unit, the first remote line 'AUX 1' (see Fig. 6) will be switched briefly to 'ON'. This signal will be scanned at the start of the suitable sample changer programs.
Terminate the program entry by activating the program with store it in the system with
Save.
Enable and
The control of the 813 Compact Autosampler is carried out similarly. The only thing to be done here is to set the remote lines to the required times as described above for each of the three working steps: auto­sampler start, pump start and pump stop in order for a brief impulse to be transferred.
In order for the connection Autosampler – 817 Bioscan to function properly the program must first be started at the sample changer and then the "Sample queue" in IC Net 2.1.
817 Bioscan
23
2 Installation

2.5 System for the analysis of anions and sugars – MIC-9

The combination of an anion system with chemical suppression with the IC system for sugar analysis is described as an example of a complete IC system for the simultaneous determination of anions and sugars.
As ideally the two sample loops for the different separation pathways should be connected by as short a piece of capillary as possible for sample injection, a 733 IC Separation Center with two injectors (2.733.0120) is used. This means that the 812 Valve Unit is no longer required for sample injection for the Bioscan. The MSM Suppressor Module, which is frequently located in the 733 IC Separation Center, is then replaced by the 753 IC Suppressor Module which is used instead of the 752 IC Pump Unit.

2.5.1 Electrical connections

The electrical connection of the system, consisting for example of two 709 IC Pumps, 817 Bioscan, 732 IC Detector, 733 IC Separation Center (2 injectors), 753 IC Suppressor Module, 762 IC Interface and 766 IC Sample Processor is made according to the Figure 9:
6.2125 .120
6.2128.130
PC
6.2134.100
6.2128.180
6.2115.070
817
709762
6.2134.090
732
733
709
753
MSM
6.2125.090
6.2141.110
6.2143.210
AB
6.2134.080
Fig. 9
: Connections with a Bioscan 817 as second detector with
a modular IC system – MIC 9
817 Bioscan
24
2.5 System for the analysis of anions and sugars – MIC-9

2.5.2 Capillary connections

This section describes the capillary connections required for the com­bination of the IC system for sugar analysis (MIC-8) with an anion sys­tem with chemical suppression (e.g. MIC-2). It is assumed that the cap­illary connections for the anion system are already known.
Arrange the necessary components as shown in Fig. 9. Please also ob­serve the recommendations about the arrangement of the IC modules given in Section 2.1.4. The capillary connections for the 817 Bioscan correspond to a large extent to the connections described in Section
2.3. Only the connection of the injection valve to the 812 Valve Unit is not necessary. Instead the second injection valve B of the 733 IC Sepa­ration Center is connected for injecting the sample for the sugar deter­mination (see below).
For the components for determination of the anions the typical ar­rangement of the capillaries for such an anion system is assumed to be present. The necessary alterations concern the injection valve A in the 733 IC Separation Center, which must be connected for injection valve B so that the two sample loops can be filled simultaneously. In addition the MSM Suppressor Module connections must be transferred to the 753 IC Suppressor Module if the 752 IC Pump Unit has previously been used with the MSM Module contained in the 733 IC Separation Center.
The necessary modifications are described below. Injections valves A and B are designated as follows:
Injection valve A: sample injection for anion determination
Injection valve B: sample injection for sugar determination
All the connections for the two injection valves are shown in Figure 10 on the following page.
1 Connection injection valve A – injection valve B
For simultaneously filling the two sample loops as short as possible piece of PEEK capillary is attached to sample outlet 48 of injection valve A and sample inlet 55 of injection valve B.
2 Connection pulsation absorber – injection valve B
Connect PEEK capillary 29 to pulsation absorber 52 in the Bioscan, lead it out through opening 2 or 3 of the Bioscan, and in through opening 27
or 28 of the 733 IC Separation Center
and connect it to injection valve B (eluent inlet 58).
3 Connection injection valve B – preheating capillary
Connect PEEK capillary at injection valve B (eluent outlet 57), lead it out through opening 27
or 28 of the 733 IC Separation Center and in through opening 2 or 3 of the Bioscan and use a PEEK coupling to connect it to preheating capillary 31.
817 Bioscan
25
2 Installation
49 48
A
51 52
Fig. 10
Injection Valve A
48 Sample outlet
PEEK capillary connection to injection valve B
49 Sample inlet
PEEK capillary connection to sample processor (18 in Instructions for Use for 766 IC Sample Processor)
: Connections of injection valves A and B
in the IC Separation Center (2.733.0120)
- Anions -
55 54
12
63
54
5350
57 58
54 Sample outlet
PTFE tubing connection to waste
55 Sample inlet
PEEK capillary connection to injection valve A
12
63
B
54
5956
Injection Valve B
- Carbohydrates -
50 Connection for sample loop
PEEK sample loop for anion analysis
51 Eluent outlet
PEEK capillary connection to anion separation column
52 Eluent inlet
PEEK capillary connection, e.g. to pulsation absorber for anion eluent
53 Connection for sample loop
PEEK sample loop for anion analysis
56 Connection for sample loop
20 µL PEEK sample loop (6.1825.210)
57 Eluent outlet
Connection of preheating capillary 31 (PEEK, 6.1836.010)
58 Eluent inlet
PEEL capillary connection 29 to pulsation absorber
59 Connection for sample loop
20 µL PEEK sample loop (6.1825.210)
817 Bioscan
26
2.5 System for the analysis of anions and sugars – MIC-9

2.5.3 Configuration in IC Net 2.1

The complete IC system is installed in IC Net using the New system
wizard
:
1 762 IC Interface
2 732 IC Detector
3 817 Bioscan
4 709 IC Pump
817 Bioscan
27
2 Installation
5 709 IC Pump
6 766 IC Sample Processor
7 733 IC Separation Center
8 753 Suppressor Module
817 Bioscan
28
2.5 System for the analysis of anions and sugars – MIC-9
9 Second data recorder
10 Anion method and data source
11 System overview
12 Final settings
In the system window of the 753 Suppressor Module the option
Start pump with hardware should be activated under Manual.
817 Bioscan
29
2 Installation
13 Bioscan method and data source
The Bioscan method and corresponding data source must be selected in the
Setup menu which can be accessed by a right-
hand mouse click on the second data recorder symbol.
14 Connect system with workplace
Under SYSTEM / Control / Connect to workplace connect the new system with the workplace.
At the same time the symbol
appears in the symbol bar.
15 Check measuring cell
If the 817 Bioscan is switched on without the flow-through cell being constantly rinsed by a conducting eluent (e.g. 0.1 M NaOH) then the measuring cell must not be switched on!
You should now check this in the instrument window of the 817 Bioscan (accessed with a double-click with the mouse on in­strument symbol) under
Manual / Cell.
16 Check connections
You can now check the electronic connections to all modules. This is done by double-clicking with the left-hand mouse key on each instrument symbol. If the connection is functioning properly then the current status of the instrument parameters will be shown.
Remarks
The event-line for the suppressor of the 753 Suppressor Module
is only set up as a "dummy connection" (Step 8). The real com­mand for switching the suppressor further is made by the 766 Sample Changer via a remote line.
For the installation described above the option
Stacked recorder icons Options / Global preferences. This is why only a symbol for the
must be activated in IC Net 2.1 under
System face /
data recorder is visible in the system overview. With a right-hand mouse click and the offered
Setup option the setting possibili-
ties described for both recorders man (Step 10 and Step 13) can be accessed.
817 Bioscan
30
2.5 System for the analysis of anions and sugars – MIC-9
Creating the time program
1. Input of the program for the 766 IC Sample Processor (Master):
001 Ctrl INIT 002 Move sample 003 Lift work 004 Ctrl ZERO 1 005 Ctrl FILL A 1 006 Ctrl STEP MSM 753 007 Ctrl FILL B/Step 1 008 Pump 120 s 009 Ctrl INJECT A 1 010 Ctrl INJECT B 1
Initialize remote interface
Move needle to sample position
Move lift with needle to working height
Trigger Autozero on 732 IC Detector
Switch injection valve A on 733 to "Fill"
Switch on 753 Suppressor-Module
Switch injection valve B on 733 to "Fill"
Fill sample loops A + B with sample for 120 s
Switch injection valve A on 733 to "Inject"
Switch injection valve B on 733 to "Inject"
1. Terminate the program entry by activating the program with and store it in the system with
Save.
Enable
2. Finally check that in the IC system the 766 Sample Processor is en­tered under
Start with inject under Setup / Start mode.
Remarks
If only one of the detection pathways is to be used in this IC system then the modules which are not required can be removed from the sys­tem (remove recorder and instrument symbols with the right-hand mouse key and
However, please note that in this instrument configuration the recording of the Bioscan data nevertheless begins only when the injection valve A on the 733 IC Separation Center is switched from is only a corresponding connection to the 762 IC Interface from this valve (see Fig. 9). This means that even if only sugar analysis is to be carried out, the 733 IC Separation Center and the 732 IC Detector must still form part of the system described above. The program described above for the 766 IC Sample Processor must then remain unchanged.
Unlink) and save the system under a new name.
Fill to Inject, as there
817 Bioscan
31
2 Installation

2.6 Preparing the 817 Bioscan for the analysis

This section describes the necessary steps for preparing the 817 Bio­scan to carry out an analysis. A more detailed description of the opera­tion of the 817 Bioscan using IC Net 2.1 can be found in Section 3 and in the ‘Instructions for Use’ of the 8.110.8221 Metrodata IC Net 2.1 software.

2.6.1 System switch-on

1 Mains on
Start up the individual instruments and the IC Net program in the following sequence:
1. Computer
2. IC instruments
3. IC Net 2.1
2 Check measuring cell
For safety reasons check the status of the measuring cell in the instrument window of the Bioscan (accessed by a double-click with the mouse on the instrument symbol) under
Manual / Cell.
If the 817 Bioscan is switched on without the flow-through measuring cell being constantly rinsed through a conducting eluent (e.g. 0.1 M NaOH) or correctly connected up then the measuring cell must not be switched on!
3 Check the external control of the 709 IC Pump
Depending on the control of the 709 IC Pump (MIC-8: manual; combination with 762 IC Interface: external) the setting of the external control of the IC Pump should be checked with key 8 <EXT.>.

2.6.2 Start pump

1 Column/ Eluent
With the Metrosep Carb 1 (6.1013.000) column use 0.1 M NaOH (quality) as the eluent for sugar analysis. This should be made up and degassed freshly every day; it should at least be de­gassed before use each day.
2 Flow rates / Pressure
The Metrosep Carb 1 column should not be subjected to large variations in pressure. For this reason each time that the eluent is used it should be pumped for a period of 10 minutes both before and after use at 0.3 mL/min. For normal operation a flow rate of1.0 mL/min is used.
Set a maximum pressure P
0.1 M NaOH this should establish a pressure of approx. 9 - 10 MPa with the Metrosep Carb 1.
817 Bioscan
32
of 15 MPa. At 1 mL/min and with
max
2.6 Preparing the 817 Bioscan for the analysis

2.6.3 Set operating mode

1 Manual control of the 817Bioscan
In the instrument window of the Bioscan (double-click with the mouse on the instrument symbol) select
Mode: Pulse for
pulse amperometric detection.
The cell must remain deactivated for as long no eluent flows through the flow-through measuring cell.
The oven is set to e.g. 32 °C. In general this temperature should be at least 10 °C higher than the ambient room tem­perature.
817 Bioscan
33
2 Installation
2 Parameters for the pulse mode
Set these method parameters for the pulse mode. Please note that this menu can only be accessed when the option
Pulse has been selected for Mode under Manual (see above).
Finally transfer the current parameters to Bioscan with < and use
System / Save to save them in the system file (*.smt).
The IC system with the 817 Bioscan is now ready for use.
Set>
817 Bioscan
34

3.1 Handling the 817 Bioscan

3 Operation

3.1 Handling the 817 Bioscan
General
Amperometric detection takes place with a flowing current and there­fore with a chemical conversion of the analyte. The course of a chemi­cal reaction depends directly on various physical parameters, among other things. In order to obtain optimum measuring conditions (e.g. stable baseline or reproducible signals) it is necessary to take the fol­lowing points into consideration. Further information can be found in Section 4.2.
Constant temperature
The 817 Bioscan allows the interior of the instrument to be kept at a constant temperature of up to max. 60°C. The lower limit is the ambient temperature plus 10 °C. Under IC Net you should activate the appropri­ate oven-operating mode in the 817 method parameters and define the temperature (see Section 3.2.2)
Constant pH
The characteristic current/potential curves of all electrochemically reac­tive substances depend very strongly on the pH of the pH eluent used. This means that you should prepare the eluent very carefully and check its pH at regular intervals.
Pulsation-free eluent flow
Changes to the eluent flow should be avoided as far as is possible. The
6.2620.150 Pulsation Absorber is available for this purpose; it is mounted between the 709 IC Pump and the injection valve as de­scribed in Section 2.3.2.
Never make dry measurements
The flow-through measuring cell must not be switched on if it is not being rinsed constantly by the eluent or if the measuring cell is not connected up properly!
817 Bioscan
35
3 Operation

3.2 Operation using «IC Net 2.1»

3.2.1 817 Bioscan icon

The 817 icon is available in the system window if an 817 Bio-
scan
has been installed with the New system wizard or by us-
ing the Setup/New devices/Install new device option of the
SYSTEM window (see section 2.4.2).
If the system is connected and the 817 icon is clicked with the right-hand mouse button then the following menu ap­pears:
Open Opens the 817 Bioscan window for parameter set-
tings (this window can also be opened by dou­ble-clicking the icon).
Unlink Deletes the 817 icon from the system.
817 Bioscan
36
3.2 Operation using «IC Net 2.1»

3.2.2 817 Bioscan window

817 icon / Open
The 817 Bioscan window for parameter settings is opened by selecting this menu option with the right-hand mouse button or by double-clicking the 817 icon in the SYSTEM window. It consists of the four tabs Manual, Method parameters, Program, and Links.
Manual
The Manual tab of the 817 Bioscan window is only available for a connected system.
817 Bioscan
Mode Selection of detector mode:
DC In the DC mode a constant potential is ap-
plied; the analytes are oxidized or reduced in accordance with their electrochemical properties.
Pulse The Pulse mode works with three different
potentials that are applied cyclically. This frees the electrode surface from any adher­ing reaction products during each sweep and an activated surface is produced for the next measurement.
Scan The Scan mode allows potential/current
curves to be recorded.
37
3 Operation
Cell Manual control of amperometric detector
cell:
<On> Switches on detector cell. <Off> Switches off detector cell.
Attention
Switch on the detector cell only if a conduct­ing eluent is being pumped through it con­tinuously!
Oven Manual control of column oven (heater):
<On> Switches on oven. <Off> Switches off oven. Temperature Temperature of column oven.
Range:
15 ... 60 °C (> room temp. + 10 °C)
Control Manual setting of 4 remote lines.
<Set> Sets remote lines to selected states. Aux1, Aux2, Cont1, Cont2
Setting of 4 remote lines. Selection:
Valve Manual switching of the injection valve,
0, 1, *
e.g. at the 812 Valve Unit:
<Fill> Switches injection valve to "Fill" position
(control line Cont1 is set to 0).
<Inject> Switches injection valve to "Inject" position
(control line Cont1 is set to 1).
Analog output
Manual setting of the analog output signal to zero. For RS232 data the full-scale range (see next page) is shifted until the signal is located in the center of this range again (s. also Chapter 6.1).
<Zero> Triggers the autozero function.
Actual
Display of actual values.
Mode Display of current detector mode. Cell Display of current cell state.
Oven
Control
817 Bioscan
38
Display of current oven state. Display of current control line settings.
3.2 Operation using «IC Net 2.1»
Method parameters
DC mode
The DC mode subtab of the Method parameters tab on the 817
Bioscan
window is used to set the parameters for the DC
mode. This window is only available if Mode has been set to
DC on the Manual tab.
Method data
Cell potential Electric potential applied to the amperomet-
ric detector cell in V Range:
Oven Switches column oven on/off and sets op-
-2 ... +2 V.
erating temperature. Range: 15 ... 60 °C (> room temp. + 10 °C)
Range Selection of measuring range:
pA 10 ... 5000 pA. nA 0.1 ... 50 nA. µA 0.01 ... 5 µA.
Full scale The full-scale range (operating range) sets
the desired sensitivity for the analog output. The possible values of the full-scale range depend on the preset measuring Range. For RS232 data (IC Net 2.1), always the maxi­mum settings should be used.
817 Bioscan
39
3 Operation
Filter Electronic damping of the analog output
(REC) and RS232 signal. Selection: 0.1, 0.2, 0.5, 1, 2, 5 s
Offset
Offset of the zero point.
Selection: -50 ... +50 % (in steps of 10 %)
Actual
Cell potential Display of current cell potential in V Oven Display of current oven state. Range Display of current measuring range. Full scale Display of current full-scale range. Filter Display of current damping constant. Offset Display of current offset.
<Set> Sends current parameters immediately to
the 817 Bioscan. Parameters are not stored in the system file (*.smt) as long as the file is not saved.
817 Bioscan
40
3.2 Operation using «IC Net 2.1»
Pulse mode
The Pulse mode subtab of the Method parameters tab on the
817 Bioscan window is used to set the parameters for the
pulse mode. This window is only available if Mode has been set to Pulse on the Manual tab.
Method data
Cell Definition of three different working poten-
tials that are applied to the amperometric detector cell cyclically. The set potentials are graphically displayed if the Method op­tion is enabled above the graphic window.
E1, E2, E3 Potentials.
Range: -2 ... +2 V.
t1, t2, t3 Time duration to apply the potentials.
Range: 0.01 ... 2 s
Sample time
Measuring time at the end of working po-
tential E1. Selection: 20, 40, 60, 80, 100 ms
Oven Switches column oven on/off and sets op-
erating temperature. Range: 15 ... 60 °C (> room temp. + 10 °C)
Range Selection of measuring range:
pA 10 ... 5000 pA. nA 0.1 ... 50 nA. µA 0.01 ... 5 µA.
817 Bioscan
In the Pulse mode, always the µA range
should be selected.
41
3 Operation
Full scale The full-scale range (operating range) sets
the desired sensitivity for the analog output. The possible values of the full-scale range depend on the preset measuring
Range. For
RS232 data (IC Net 2.1), always the maxi­mum settings should be used.
Offset Offset of the zero point.
Selection: -50 ... +50 % (in steps of 10 %)
Actual
E1, E2, E3 Display of current potentials in V. t1, t2, t3 Display of current time durations for poten-
tials in s.
Sample time Display of current sample time in ms. Oven Display of current oven state. Range Display of current measuring range. Full scale Display of current full-scale range. Offset Display of current offset.
Cycle potentials Graphical display of cycle potentials.
Method Display of potentials set in the Method data
frame.
Actual Display of current potentials.
<Set> Sends current parameters immediately to
the 817 Bioscan. Parameters are not stored in the system file (*.smt) as long as the file is not saved.
817 Bioscan
42
3.2 Operation using «IC Net 2.1»
Scan mode Parameters
The Scan mode subtab of the Method parameters tab on the
817 Bioscan window is used for parameter setting and curve
display for the scan mode. This window is only available if
Mode has been set to Scan on the Manual tab.
Method data
Cell potential Definition of start and end potential for a
user-defined potential sweep that is applied to the amperometric detector cell.
E1 Start potential for sweep.
Range: -2 ... +2 V.
E2 End potential for sweep.
Range: -2 ... +2 V.
Scan cycle Definition of scan cycle:
full double scan E1 ... E2 ... E1 half single scan E1 ... E2 Selection: full, half
Scan rate Definition of scan rate in mV/s.
Selection: 1, 2, 5, 10, 20, 50 mV/s
Oven Switches column oven on/off and sets op-
erating temperature. Range: 15 ... 60 °C (> room temp. + 10 °C)
Range Selection of measuring range:
pA 10 ... 5000 pA. nA 0.1 ... 50 nA. µA 0.01 ... 5 µA.
817 Bioscan
43
3 Operation
Full scale The full-scale range (operating range) sets
the desired sensitivity for the analog output. The possible values of the full-scale range depend on the preset measuring
Range. For
RS232 data (IC Net 2.1), always the maxi­mum settings should be used.
Offset Offset of the zero point.
Selection: -50 ... +50 % (in steps of 10 %)
Actual
E1, E2 Display of current start and end potentials
in V.
Scan cycle Display of current scan cycle mode. Scan rate Display of current scan rate in mV/s. Oven Display of current oven state. Range Display of current measuring range. Full scale Display of current full-scale range. Offset Display of current offset.
<Set> Sends current parameters immediately to
Scan mode Operations
the 817 Bioscan. Parameters are not stored in the system file (*.smt) as long as the file is not saved.
817 Bioscan
44
3.2 Operation using «IC Net 2.1»
Caption Possibility of entering a title that is written
at the head of the scan mode graphics window.
Program
<Add date & time>
The current date and time are added to
the title defined in the Caption field.
State Display of current state. <Start> Starts scan mode sweep. <Stop> Stops scan mode sweep.
<Copy to clipboard> Copies the content of the scan mode
graphics window to the clipboard.
On the Program subpage, program steps including time, program instruction and parameter can be entered.
First 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 to-
gether with the last instruction with time entry.
Second column Program instruction (see below). Third column Parameter for program instruction (see
below).
ENABLED Enable program start (a disabled pro-
gram 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).
817 Bioscan
45
3 Operation
List of program instructions
The following program instructions can be added to the time program on the
Program subpage:
Instruction Parameter entry Meaning
Mode DC, Pulse, Scan
Cell On, Off Switch cell on/off.
Outputs 0, 1, * Set remote lines Aux1, Aux2, Cont1
Select detector mode.
and Cont2 to desired values. For entry of the first value, enter
1, 0 or *. For
entry of the other values, move the cursor in front of the value to be changed and enter
Range pA: 10 pA – 5 nA
nA: 0.1 nA – 50 nA µA: 10 nA – 5 µA
Offset -50, -40, -30,…50 % Set offset for measuring signal.
Valve Fill, Inject Switch connected injection valve.
Oven off, 15 ... 60 °C Set column oven temperature.
Autozero Trigger analog output signal auto
Set measuring range.
1, 0 or *.
zero.
DC_E -2 ... +2 V Set measuring potential (DC).
Filter 0.1, 0.2, 0.5 ... 5 s Set electronic damping for the
analog output signal.
Scan_E1 -2 ... +2 V Set sweep start potential E1.
Scan_E2 -2 ... +2 V Set sweep end potential E2.
Scan_Cycle half, full Select scan cycle type.
Scan_Rate 1, 2, 5, … 50 mV/s Set scan rate.
Links
The Links tab of the 817 Bioscan is used for COM port selec­tion and settings (details see Section 5.2.4 in the Software Manual for IC Net 2.1).
817 Bioscan
46
4.1 Introduction

4 Basic principles

4.1 Introduction

The 817 Bioscan can be operated as an amperometric detector in three different working modes:
DC mode A constant potential is applied to the working elec-
trode. The analyte substances are oxidized or re­duced according to their electrochemical properties. The current that is produced is measured.
Scan mode Current-potential curves are recorded in order to de-
termine the optimum parameters for pulsed am­perometric detection. This is done by passing a so­lution that contains only the substance of interest through the measuring cell and recording a current­potential curve.
Pulse mode Three different potentials are applied cyclically to
the working electrode. This frees the electrode sur­face from any adhering reaction products and reac­tivates it for the next measurement. As this is the operating mode that is primarily used with the 817 Bioscan for carbohydrate analysis it is described in detail in Section 4.2.
817 Bioscan
47
4 Basic principles

4.2 Measuring conditions

Amperometric detection takes place with a flowing current and there­fore with a chemical conversion of the analyte. The course of a chemi­cal reaction depends directly on various physical parameters, among other things. In order to obtain optimum measuring conditions (e.g. stable baseline or reproducible signals) it is necessary to take the fol­lowing points into consideration:
Temperature The reactions occurring at the working electrode
(oxidation and reduction) are influenced by the tem­perature. However, this applies not only to the con­version of the analyte, but also for interfering reac­tions that produce the background current. This is the reason why a constant temperature is a neces­sary precondition for obtaining a stable baseline and reproducible signals. For the determination of carbohydrates, lower temperatures (30 °C – 35 °C) are suitable. Furthermore, the flowcell should not be operated above 45 °C over a longer time period.
pH Just like the temperature, the pH of the eluent also
has a direct influence on the electrochemical reac­tions at the working electrode. pH alterations cause a displacement of the characteristic current/poten­tial curves (voltammograms). Possible results are the reduction of the signal intensity and lower sig­nal/noise ratios. In order to ensure that a stable baseline and reproducible measuring conditions are obtained care should be taken that the pH of the eluent is correct.
Pulsation Electrochemical reactions at the electrode surfaces
depend on the transport of the reacting substances to the electrode. This is why a constant eluent flow is crucial, both for a stable baseline and also for re­producible signals. This is why pulsation-free eluent supply must be ensured. You should use the pulsa­tion absorber provided (see Section 2.3.2).
817 Bioscan
48

4.3 Pulsed amperometric detection

4.3 Pulsed amperometric detection
During an amperometric determination the reaction products formed on the working electrode can alter its surface properties by adsorption. In pulsed amperometric detection (PAD) it is possible to apply further po­tentials cyclically in addition to the detection potential in order to ensure a constant electrode surface. In this way the electrode surface is re­newed after each current measurement and remains in this activated condition.
The exact potential steps are shown in Fig. 11 as a function of time.
Fig. 11: Potentials applied during pulsed amperometric detection (PAD)
The working potential E1 is applied during the time t1 with the signal being measured in ts. The high positive potential E2 causes the oxida­tive removement of reaction products from the electrode surface, which is reduced to a pure Au-surface during t3.

4.3.1 Optimization of the PAD parameters

When adapting the method parameters the preset parameters should initially be used. Descriptions of various applications are available from Metrohm AG in the form of Application Works and Application Notes. These can be obtained from your local Metrohm agency or on the Inter­net under www.metrohm.com
The potential profile shown in Fig. 11 must always be matched to the analyte under investigation. 7 parameters must be taken into account: potentials E1, E2 and E3, time intervals t1, t2 and t3 and the measuring time ts. Some basic conditions are preset; this makes configuration easier. These are described below.
.
2.0 1.0
817 Bioscan
49
4 Basic principles
Measuring interval (E1, t1 and ts)
The measuring potential depends on the substance being investigated. If no data is available in the literature that can initially be used for opti­mization then you can determine these parameters yourself. For this reason Bioscan has the scan mode available, among other things. Re­cording the corresponding voltammograms is described in Section 4.4.
As each change in potential can cause a higher charging current to oc­cur at the working electrode, the current measurement itself is only started when the signal has stabilized itself to a large extent. This time is defined as t1 – ts (see Fig. 11). It influences the level of the back­ground current and should therefore be selected so that it is not too small. In practice a time of 0.1 to 0.4 s is frequently used.
The measuring interval ts can be set to 20, 40, 60, 80 or 100 ms. These values correspond to multiples of 50 Hertz. In this way possible interfer­ence from the mains current supply can be avoided.
Regeneration interval (E2, E3, t2 and t3)
The potentials E2 and E3 which are required for the regeneration of the electrode surface are primarily determined by the material of the work­ing electrode.
With the gold electrode used the oxide layer is already formed at E2 > +200 mV (Ag/AgCl) under alkaline conditions. Higher potentials accel­erate oxide formation, therefore in practice E2 = +750 mV and t2 = 0.2 s are often selected.
For example, –800 mV at 0.2 s or –150 mV at 0.4 s can be selected for E3 and t3.
Measuring frequency
In pulsed amperometric detection the total of the three individual inter­vals (t1 + t2 + t3) represents the duration of one measuring cycle. The reciprocal of this cycle duration (in seconds) gives the pulse fre- quency. Please note that the measured value is outputted from the de­tector at this pulse frequency. The sampling frequency which other­wise has to be set under IC Net for data acquisition (
M
ethod setup / Measure / Sampling rate and Frequency divisor) is
automatically adapted accordingly.
IC NET / Method /
817 Bioscan
50

4.4 Optimization of the measuring potential

4.4 Optimization of the measuring potential
An optimization of the measuring potential for amperometric detection may bring benefits in the following situations:
a) The sensitivity of the detection of the analyte is to be increased
against the background signal.
b) The selectivity of the detection is negatively affected by the analyte
peak overlapping with a second substance peak that has not been optimally separated by chromatography.
If there are no suitable literature data available, this requires the re­cording of a voltammogram. This is a curve showing the relationship between the given potential and the measured current. It is characteris­tic for individual chemical substances or even whole classes of sub­stances.
There are two different types of voltammograms, each of which is suit­able for solving a different problem: a hydrodynamic voltammogram and a scan voltammogram.
Fig. 12
A hydrodynamic voltammogram is made of several chromatograms recorded in the DC mode. This involves recording a chromatogram of the substance under investigation, dissolved in eluent, at a constant po­tential. The potential is now varied several times and the process is re­peated. Finally the height of the current peak obtained is evaluated and plotted against the particular potential. Fig. 12 shows a schematic ex­ample of such a hydrodynamic voltammogram:
I
: Example of a hydrodynamic voltammogram of a substance (A)
with the additional presentation of the measured values for the pure eluent (B)
817 Bioscan
This method is advantageous if the analyte is not present in a pure form. It also provides more realistic information about the signal/noise ratio and the selectivity towards overlapping peaks.
51
4 Basic principles
The scan voltammogram is recorded in the scan mode. The measur­ing potential is varied backwards and forwards between two given limits while the analyte is passed through the measuring cell. The actual cur­rent is then measured for each potential.
The substance under investigation can be dissolved in the IC eluent used (e.g. 10 ppm Sucrose in 0.1 M NaOH) and a larger amount (e.g. 100 mL) pumped through the flow cell without a separation column connected. If you work on trace concentrations of your analyte and worry about contamination of your IC system you can still inject the substance into the eluent using a large sample loop (> 500 µL). The eluent should then be pumped at a very low flow rate (e.g. 0.05 mL/min).
In principal, same conditions should be used as they are needed for the chromatographic separation (e.g. temperature, pH, eluent etc.).
Fig. 13 shows a schematic example of a scan:
Fig. 13
: Example of a scan of a substance (A) with the additional repre-
sentation of the scan of the pure eluent (B)
When using metal electrodes as the working electrode, such as the gold electrode used here, the reaction products formed by the am­perometric detection during the scan method can form an interfering layer on the electrode surface and influence the results. For this reason a hydrodynamic voltammogram is to be preferred in such cases.
The following table summarizes the requirements for and the advan­tages and disadvantages of these two methods.
817 Bioscan
52
4.4 Optimization of the measuring potential
Situation
Requirement
Advantages
Disadvantages
Hydrodynamic
voltammogram
Selectivity for an inadequate IC-separation is to be im­proved
Substance can be investi­gated in the mixture
IC parameters must be known
"Chromatographic" condi­tions, i.e. a direct check of selectivity and sensitivity is possible
Several substances can be investigated at the same time
More time required for a single substance
Scan
voltammogram
Sensitivity of a substance peak is to be increased
Substance must be present in a pure form
Less time needed for single substances
Possible formation of an oxide layer on the working electrode
The final aim is to select a suitable potential for use as the measuring potential for pulsed amperometric detection. This means that usually a compromise has to be found between the highest possible sensitivity, selectivity and reproducibility:
Higher potentials can increase the sensitivity; however, more sub­stances can also be determined and this reduces the selectivity. In or­der to achieve high reproducibility, a potential from a flatter segment near to the maximum of the analyte voltammogram should be selected. In the example shown in Fig. 12, E
was a potential determined in this
1
way.
During the determination of the optimum measuring potential the constancy of the parameters pH and temperature as well as the pulsation-free eluent supply are important (see Section 4.2).
817 Bioscan
53
4 Basic principles
817 Bioscan
54

5.1 Practical notes on ion chromatography

5 Notes – Maintenance – Faults

5.1 Practical notes on ion chromatography

5.1.1 Separating columns

Separation efficiency
The attainable quality of analyses with an IC system 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. Compare the standard chro- matogram enclosed with the column with your own measurements. If any difficulties arise, you should always first check the quality of the column by recording a standard chromatogram.
You will find additional detailed information on the separating columns available from Metrohm in the leaflets supplied and in the Application Works and -Notes, which are available on request free of charge at 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.
To avoid contamination by abrasive particles arising from piston seals of the high-pressure pump, it is advantageous to install an in-line filter between the pump and the injection valve. The 6.2821.100 Filter unit PEEK is best suited for this purpose. It is a part of the standard equip­ment of the 709 IC Pump.
Storage
Always store the separating columns closed and filled when not in use in accordance with the manufacturer’s specifications.
817 Bioscan
55
5 Notes – Maintenance – Faults
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 (see sec- tion 6.3.2), 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,

5.1.2 High-pressure pump

Pulsation absorber
For determinations using the Bioscan pulsation-free high-pressure pumps with very constant flow rates are needed. However, if pulsation is too high, the use of the 6.2620.150 Pulsation dampener MF is rec- ommended. It is also used to protect the column material against pres­sure shocks caused by the injection. Its installation is described in sec- tion 2.3.2.
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. When the cleaned valves are reinstalled, you must ensure that the flow direction is correct.
The replacement of piston seals has to be done in accordance with the pump manufacturer’s directions. The corresponding maintenance work for the 709 IC Pump is described in section 4.2 of the 709 Instruc- tions for Use.
Salt crystals between the piston and the seal are the cause of abrasive particles, which can enter the eluent. These lead to contaminated valves, pressure rise and in extreme cases to scratched pistons. It is thus essential to ensure that no precipitates can appear (see also section 5.1.3).
817 Bioscan
56
5.1 Practical notes on ion chromatography

5.1.3 Eluents

Treatment
For the preparation of the eluents only chemicals of a purity degree of at least "p.a." should be used. For diluting please use only high purity water.
Fresh eluents should always be microfiltered (0.45 µm filter) and de- gassed (with N eluent should be continuously stirred with a magnetic stirrer, particu­larly when the recycling procedure is employed or when alkaline eluents are used. For alkaline eluents and eluents with low buffering capacity one should preferably use a CO with the optional 6.5324.000 Bottle rack).
The supply vessel containing the eluent must be closed as tightly as possible to avoid excessive evaporation. 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.
, He or vacuum). For high sensitive measurements, the
2
absorber (e.g. the absorber supplied
2
Influence of various parameters on separation columns
Concentration: An increase in the concentration usually leads
pH: pH alterations lead to shifts in the dissociation
Eluent change
When the eluent is changed, it must be ensured that no precipitates can be formed. Solutions used in direct succession must therefore be miscible. If the system has to be rinsed with an organic solution, several solvents with increasing or decreasing lipophilic character may possibly have to be used (e.g. water acetone chloroform).

5.1.4 Connections

All connections between injector, column and detector must be as short as possible, have a low dead volume and be absolutely tight.
to shorter retention times and quicker separation, but also to a higher background conductivity.
equilibrium and thus to changes in the retention times.
817 Bioscan
57
5 Notes – Maintenance – Faults

5.2 Maintenance and servicing

5.2.1 General information

Care
The 817 Bioscan requires proper care and attention. Excessive con­tamination of the instruments 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 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 1.4.1.
In the electronic compartment of the 817 Bioscan a lithium battery is mounted. If this unit or battery needs service, dispose it according to chemical waste only.
Maintenance by Metrohm service
Maintenance of the IC system 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.

5.2.2 Shutdown

If the IC System is shut down for a considerable length of time, the en­tire IC system (without methanol/water (1:4) to avoid crystallization of eluent salts with the cor­responding subsequent damage.
column) must be rinsed free from salt with
For rinsing the separating column module is removed and bridged. The flowcell must be turned off Rinse with methanol/water (1:4) until the conductivity of the eluent drops below 10 µS/cm.
817 Bioscan
58
5.2 Maintenance and servicing

5.2.3 Cleaning the working electrode

The surface of the gold working electrode should be cleaned whenever you notice that its electrochemical properties have changed. This may be caused by the deposition of reaction products. High current flows can also alter the electrode surface; this is indicated by a very reduced sensitivity after longer periods of use.
In principle, you should avoid too high analyte concentrations or dirty samples. This measure as well as the regenerative effect of the pulse technique normally supersedes the polishing of the electrode.
You should only polish the electrode surface with the polishing paste supplied when the sensitivity cannot be restored by intensive rinsing of the flowcell with water and cleaning the electrode surface with a tissue soaked in ethanol or acetone.
Use the diamond paste (6.2802.110) supplied to polish the surface of the electrode together with the polishing disk (6.2802.100). Proceed as follows:
1 Rinse the polishing disk
Rinse the polishing disk with water (distilled or deionized) before use.
2 Shake the diamond paste
Shake the bottle containing the diamond paste thoroughly before use.
3 Polish the electrode
Add a few drops of the paste to the wet paste to the wet polish­ing disk and polish the electrode for approx. one minute with uniform movements in the form of a figure 8. Exert only a slight pressure.
4 Clean the electrode
Clean the electrode with a paper tissue moistened with ethanol. Check the surface condition visually and repeat the polishing process if necessary.
5 Mount the flow-through cell
Remount the detector cell as described in Section 2.3.5. Pay attention to an exact fitting of the spacer, the right position of both markers 35, and a correct screw joint (s. section 2.3.5).
817 Bioscan
6 Clean the polishing disk
Clean the polishing disk with water (distilled/deionized) and store it dust-free in its plastic cover.
59
5 Notes – Maintenance – Faults

5.2.4 Changing separating columns

Identical separation system
If you wish to replace an IC separating column by a column of the same type, proceed as follows (see Fig. 3):
1 Remove old column
Switch off flowcell.
Switch off pump drive of the 709 IC Pump.
Unscrew connection capillary 21 to flowcell from the column.
Unscrew preheating capillary 31 from column.
2 Connect new column to injector
Remove end caps from column.
Screw preheating capillary 31 to inlet end of separating
column (note flow direction).
3 Rinse column
Place beaker beneath the column outlet.
Switch on 709 IC Pump and rinse column with eluent for ca.
10 min with 0.3 mL/min and for ca. 50 min. with 1.0 mL/min, then switch off pump.
4 Connect column to flowcell
Screw connection capillary 21 to flowcell to outlet end of separating column.
817 Bioscan
60

5.3 Faults and malfunctions

5.3 Faults and malfunctions

5.3.1 Malfunctions and their rectification

If difficulties appear with the IC system during analyses, their causes are best investigated in the order separating column pump eluent 817 Bioscan. Several of the malfunctions which may appear are listed in the following table with details of possible causes and countermeasures.
Malfunction Cause Rectification
Baseline with high noise level, pulsation
Drift of the baseline
Decreasing sensitivity (S/N lower)
Contaminated pump values
Faulty piston seals
Quality of the pump
does not suffice for the selected sensitivity
Air bubble in flowcell
Temperature fluctuation
Working electrode
contaminated
Flowcell leakage
Eluent contaminated
Thermal equilibrium not
yet reached
Leak in system
Old Eluent (too much
CO2)
Working electrode contaminated, e.g. by contaminated sample
Wrong measuring potential
Eluent contaminated (high background signal)
Eluent pH changed
Clean the valves (see
section 5.1.2)
Replace the piston seals
(see section 5.1.2)
Use pulsation dampener, use more powerful pump or lower the sensitivity
Remove air bubble, degas eluent continuously
Isolate flowcell or switch on 817 Bioscan oven
Clean working electrode (see Chapter 5.2.3)
Check capillary connec­tions at flowcell
Replace eluent
Condition system with
heating switched on
Check connections and make leakproof
Replace eluent
Clean working electrode
(see Chapter 5.2.3), dilute sample
Optimize measuring potential
Replace eluent
Check and adjust pH
817 Bioscan
High background signal
Eluent contaminated
Wrong measuring
potential / pulse settings
Very broad peaks due to retarded compounds
Separation column is bleeding
Replace eluent
Optimize parameter
Await complete elution of
these compounds
Replace column
61
5 Notes – Maintenance – Faults
Signal "overload" Wrong IC-Net parameter
Range' and 'Fullsca-
'
le
'
Damaged reference electrode
Damaged working electrode
Flow cell is not con­nected properly
Wrong measuring potential
Considerable pressure drop
Considerable pressure rise
Leak in system Check connections and
Contamination of the
filter in the 6.2821.100 Filter unit PEEK
Change of column packing by injection of contaminated samples
Mounting screws flow cell overtighten; 25 µm spacer has been used
36 of
Check settings
Check and replace
reference electrode
Replace working electrode
Check cable connections
(REF: black, WE: red, AUX: blue)
Optimize measuring potential
make leakproof
Replace the 6.2821.110 Filter
Regenerate the column (see section 5.1.1) or replace column
:
Note Samples should always be microfiltered.
Check screws of flowcell; use 50 µm spacer
Chromatograms with poor resolu­tion, change in the retention times
Extreme peak broadening, splitting (double peaks)
No signal from detector
Deterioration in separation efficiency of the IC column
Old Eluent
Ionic strength or pH of
the sample differs strongly from eluent
Dead volume at the column ends
Dead volume in IC system
No mains current
817 Bioscan not
switched on
Faulty fuse
Incorrect mains voltage
Measuring cell not
connected
Dirty working electrode
Connection to IC Net is
not working properly
Regenerate the column
(see section 5.1.1) or replace column
Replace eluent
Dilute sample or change
pH of sample
Replace column
Check connections
Check mains supply and
voltage (see Section 2.2)
Switch on the 817 at the rear panel
Replace fuse (see section
2.2.1)
Check mains voltage (see Section 2.2.1)
Check connection
Clean working electrode
(see Section 5.2.3)
Check connection
817 Bioscan
62

5.4 Instrument test with the dummy cell

5.4 Instrument test with the dummy cell
If any interference occurs whose source is suspected to lie in signal re­cording or transfer you can selectively check the instrument electronics and the connection to the PC. This is done by connecting the
6.2813.030 Dummy Cell supplied instead of the built-in flow-through measuring cell. The temperature in the 817 Bioscan should be kept constant (30 °C) and, for optimal shielding, the front door should be closed.
This dummy cell contains a resistor (300 M) and a condenser (0.47 µF) connected in parallel. If a voltage of 0.8 V is applied in the DC mode then a current of 2.67 nA (± 1%) is measured at this cell. The condenser functions as a noise generator and simulates the capacitance of a well­functioning measuring cell.
Please make the following settings in IC Net:
817 Bioscan
If you use these settings to record a baseline (
ware (Measure baseline
nA. Even at maximum magnification the noise should not exceed 0.01 nA.
)) you should see a smooth signal line at 2.67
Control / Startup hard-
63
5 Notes – Maintenance – Faults

5.5 Validation / GLP

The requirements of GLP (Good Laboratory Practice) include a peri- odic check of analytical measuring instruments with regard to their re­producibility and accuracy using Standard Operating Procedures, SOP.
Further information on the subjects of QA, GLP and validation can also be found in the brochure «Quality management with Metrohm», which is available from your local Metrohm agency.
The 817 Bioscan as part of a complete IC system, whose most impor­tant components also include separating column, pump and evaluation system, must be incorporated in its comprehensive validation.
Testing of the electronic and mechanical function groups of Metrohm instruments can and should be performed as part of a regular service by trained personnel of the manufacturing company (see section 5.2.1). All Metrohm instruments are equipped with start-up-test routines that check for perfect functioning of the relevant assemblies when the in­strument is switched on.
The Metrohm company also supplies its instruments with an integrated diagnostic feature (see section 5.4) which, in the case of possible mal­functions or faulty behavior, allows the user to check the functioning of certain assemblies and localize the fault. Diagnostic programs can also be integrated in a validation procedure.
817 Bioscan
64
6.1 Technical data

6 Appendix

6.1 Technical data

Measuring unit
Operating modes DC, Pulse and Scan
Potential Range: -2.00 ...+ 2.00 V
Resolution: 10 mV
Operating modes
DC mode Range: 10 pA – 5 µA
Resolution: 1,2,5 Steps
Pulse mode Range: 10 nA – 5 µA
Resolution: 1,2,5 Steps
Pulse times: t1: 0.1 – 2.0 s t2: 0.1 – 2.0 s t3: 0 (off) – 2.0 s Resolution: 10 ms
Sample times: 20, 40, 60, 80 and 100 ms
Scan Range: 10 nA – 5 µA
Resolution: 1,2,5 Steps
Scan rate.: 1 – 50 mV/s Resolution: 1,2,5 Steps
Cycle: half, full
817 Bioscan
Autozero
Function Shift of full scale window of RS232 data;
automatic zero setting (electronic background compensa­tion) of the analog output
16 µA in µA range 160 nA in nA range 16 nA in pA range
Initiation Externally (RS232, Remote)
65
6 Appendix
Measuring cell
Construction Flowcell with working electrode, reference electrode and
auxiliary electrode; don't run above 45 °C over a longer time period
Cell volume spacer cell volume
25 µM 0.15 µL 50 µM 0.29 µL 120 µM 0.71 µL
Oven
Temperature range Accuracy Stability
Mains connection
Voltage 110 - 120 V / 220 – 240 V
Frequency 50...60 Hz
Power consumption 150 VA
Fuse 5 mm Ø, 20 mm length
RS 232 Interface
Connector Dsub 25 pin (female)
Default settings 9600 baud, 8 bit, 1 stop bit, no parity,
10 °C above ambient to 60 °C
0.5 °C
0.1 °C
Switching with mains voltage selector in fuse holder (see section 2.2.1)
100120 V: 3.15 A (slow-blow) 220240 V: 1.6 A (slow-blow)
hardware handshake
Remote lines
Remote output 4 lines at upper remote connections 15,
supportet by IC Net 2.1 (see section 2.4.3)
'AUX 1' and 'AUX 2'
Relay 1 and relay 2
max. 28 V(DC), 250 mA
1
maximum load: 28 V, 500 mA
2
66
817 Bioscan
6.1 Technical data
Signal output
I = I + I + I
Azero Offset
cell ADC Azero offset
Icell RS232
Cell
IE convertor
ADC CPU DAC REC
INT
RS232 INT REC
output signal
+/- 21 µA ( with comp.)
+/- 10 V +/- 1V
Max. range 5 nA, 50 nA, 5 µA * idem idem
Max. comp. 16 nA, 160 nA, 16 µA idem idem
Max. signal 21 nA, 210 nA, 21 µA idem idem
Resolution 1 pA, 10 pA, 1 nA Unlimited,
12 bits (0.5 mV) purely analogue (only limited by acquisition software)
Auto zero Resets zero point of
Set to 0 V Set to 0 V
full scale window **
Offset Resets full scale
window to % of full
Set relatively to subrange setting
Set as % of full scale
output
scale range ***
817 Bioscan
Filter
Y N Y
(DC only)
* In RS232 data acquisition use always the maximum range settings. Minor
range settings do not amplify the signal, however they limit the full scale. Minor range settings affect (amplify) the REC output only.
** If a 5 µA range setting is used, the full scale window is –5..+5 µA.After auto
zero at a background current of 1 µA and, this full scale window is –4..+6 µA.
*** If a 5 µA range setting is used, the full scale window is –5..+5 µA. Applying –
50% offset, results in a full scale window of –2.5..+7.5 µA.
67
6 Appendix
Safety specifications
Construction / testing According to IEC61010-1 / EN 61010-1
Safety directions The Instructions for Use include information and
warnings to which the user must pay attention in order to assure safe operation of the instrument.
Electromagnetic compatibility (EMC)
Electromagnetic compatibility Standards met:
EN61326-1
Emission Standards met:
EN55022 (class B), EN61000-3-2, EN61000-3-3
Immunity Standards met:
EN61000-4-2, EN61000-4-3, EN61000-4-4, EN61000-4-5, EN61000-4-6, EN61000-4-11
Ambient temperature
Nominal operating range +5+45°C
(at 2080 % atmospheric humidity)
Storage, transport –40+70°C
Housing
Material of cover Polyurethane rigid foam (PUR) with fire protection
for fire class UL94VO, CFC-free
Material of base Steel, enamelled
Width 260 mm
Height 385 mm
Depth 343 mm
Weight 17.9 kg (without accessories)
68
817 Bioscan
6.2 Standard equipment

6.2 Standard equipment

Subject to changes! All dimensions are given in mm.
The 2.817.0010 Bioscan includes the following parts:
Quant. Order No. Description
1 1.817.0010 Bioscan
1 6.1831.010 PEEK Capillary
Length = 3 m
0.25
1
"
1 6.1836.010 Preheating capillary
Länge = 3 m
1 6.1254.010 Au-Flowcell for 817
Three-electrode-flowcell for am­perometric detection; with working electrode, auxiliary electrode and reference electrode
2 connections for
2 6.1254.020 Spacer 50 µM
Spacer disk for 6.1254.010 flowcell; defines cell volume
1 6.2125.150 Adapter
25 pin (male./male)
For connection of 6.2125.160 RS cable to Bioscan RS 232 interface
1
16" capillaries
1 6.2125.160 Cable
Connecting cable 817 Bioscan (RS 232 interface) – PC
25 pol.
5 m
9 pol. neg.
817 Bioscan
2 6.2140.030 Conn. block 12 pols for 817
for connection of single remote cables to remote connection and
15
1 6.2156.000 Cable for 6.1254.010 Flowcell
Connection of 6.1254.010 Flowcell to detector controller
12
69
6 Appendix
Quant. Order No. Description
1 6.2620.150 Pulsation absorber MF
Metal-free pulsation absorber to reduce pulsations and prolong the life of separating columns.
52
1 6.2744.010 PEEK compression fitting
For the connection of 6.1831.010 PEEK capillaries or 6.1822.010 PTFE microcapillaries, set of 5
1 6.2744.014 PEEK compression fitting
For the connection of 6.1831.010 PEEK capillaries or 6.1822.010 PTFE microcapillaries, set of 2
1 6.2744.040 PEEK coupling
for the connection of capillaries
4 6.2744.130 Compression fitting for 6.1254.010
Connection of
1 6.2802.100 Polishing disk
For polishing the Au-working electrode of the 6.1254.010 flowcell
1
16"
1
16" capillaries to flowcell
9.5
76
26
26
24
1 6.2802.110 Diamond slurry 1 µm 10 mL
For polishing the Au-working electrode of the 6.1254.010 flowcell with the
6.2802.100 polishing disk
1 6.2813.030 Dummy cell for 817
For testing the detector control and data acquisition
1 6.6034.013 IC Net 2.1 CD
1 8.817.1003 Instructions for Use (English)
for 817 Bioscan
Optional assessories
Quant. Order No. Description
1 6.2141.140 Cable
Remote connection 817 Bioscan – Sample Processor 766/788/813
70
817 Bioscan

6.3 Warranty and conformity

6.3 Warranty and conformity

6.3.1 Warranty

The warranty on our products is limited to defects that are traceable to material, construction or manufacturing error which occur within 12 months from the day of delivery. In such cases the defects will be recti­fied in our workshops free of charge. Transport costs are to be paid by the customer.
For day and night operation the warranty is limited to 6 months.
Glass breakage in the case of electrodes or other parts is not covered by the warranty. Checks which we are asked to carry out during the warranty period for reasons other than material or manufacturing faults will be invoiced. For parts manufactured by third parties, insofar as these constitute an appreciable part of our instrument, the warranty stipulations of the manufacturer in question apply.
With the regard to the guarantee of accuracy, the technical specifica­tions in the instruction manual are authoritative.
With regard to defects in material, construction or design as well as the absence of guaranteed features, the purchaser has no rights or claims except those mentioned above.
If damage of the packaging is evident on receipt of a consignment or if the goods show signs of transport damage after unpacking, the carrier must be informed immediately and a written damage report demanded. Lack of an official damage report releases Metrohm from any liability to pay compensation.
If any instruments and parts have to be returned, the original packaging should be used if at all possible. This applies above all to instruments, electrodes, burette cylinders and PTFE pistons. Before embedding them in wood shavings or similar material, the parts must be packed in a dustproof package (for instruments the use of a plastic bag is impera­tive). If open assemblies are enclosed in the scope of delivery that are sensitive to electromagnetic voltages (e.g. data interfaces etc.) these must be returned in the associated original protective packaging (e.g. conductive protective bag). (Exception: assemblies with built-in voltage source belong in a non-conductive protective packaging).
For damage which arises as a result of non-compliance with these in­structions, no warranty responsibility whatsoever will be accepted by Metrohm.
817 Bioscan
71
6 Appendix

6.3.2 EU Declaration of Conformity

EU Declaration of Conformity
The company Metrohm AG, Herisau, Switzerland, certifies herewith, that the following instrument:
817 Bioscan
meets the CE mark requirements of EU Directives 89/336/EWG and 73/23/EWG.
Source of specifications:
EN 61326-1 Electromagnetic compatibility
EN 61010-1 Safety requirements for electrical equipment
for measurement, control and laboratory use
Description of apparatus:
Pulsed-amperometric detector for ion chromatography;
with oven and analog-digital converter
Herisau, May 3, 2001
Dr. J. Frank Ch. Buchmann
Development Manager Production and Quality Assurance Manager
72
817 Bioscan
6.3 Warranty and conformity

6.3.3 Certificate of Conformity and System Validation

Certificate of Conformity and System Validation
This is to certify the conformity to the standard specifications for electrical appli­ances and accessories, as well as to the standard specifications for security and to system validation issued by the manufacturing company.
Name of commodity: 817 Bioscan
System software: Stored in ROMs
Name of manufacturer: Metrohm Ltd., Herisau, Switzerland
This Metrohm instrument has been built and has undergone final type testing according to the standards:
Electromagnetic compatibility: Emission EN55022 (class B), EN61000-3-2, EN61000-3-3
Electromagnetic compatibility: Immunity EN61000-4-2, EN61000-4-3, EN61000-4-4, EN61000-4-5, EN61000-4-6, EN61000-4-11
Safety specifications IEC61010-1, EN61010-1
The technical specifications are documented in the instruction manual.
The system software, stored in Read Only Memories (ROMs) has been validated in connection with standard operating procedures in respect to functionality and performance. The features of the system software are documented in the instruc­tion manual.
Metrohm Ltd. is holder of the SQS-certificate of the quality system ISO 9001 for quality assurance in design/development, production, installation and servicing.
Herisau, May 3, 2001
Dr. J. Frank Ch. Buchmann
Development Manager Production and Quality Assurance Manager
817 Bioscan
73
6 Appendix
74
817 Bioscan
6.4 Index

6.4 Index

817 Bioscan
Handling ..........................................35
Installation........................................ 11
Opening ............................................. 9
Preparation ......................................32
Standard equipment........................ 69
A
Abrasive particles ................................56
Actual ...................................................38
<Add date & time> ..............................45
<Add> .................................................45
Allen key............................................... 17
Ambient temperature......................35,68
Amperometric detection ...................... 48
Analog output ....................................... 38
Analog signal (Int.) 8
Figure.................................................4
Analog signal (REC.) 7
Figure.................................................4
Appendix.............................................. 65
Application Notes .............................7,55
Application Works................................ 55
Arrangement of the instruments..........12
Aspirating filter (6.2821.090)
Notes................................................55
Aspirating Filter (6.2821.090) ..............56
Aspiration tubing connection 43
Figure............................................... 16
Autozero............................................... 65
Auxiliary electrode connection 39
Figure............................................... 17
B
Background current............................. 48
Background signal high ......................61
Baseline ...............................................35
Baseline with high noise level.............. 61
Basic principles ...................................47
Battery.................................................. 58
Bottle rack (6.5324.000)
Connection ......................................15
C
Cable connection 27
Figure.................................................6
Capillary connections ..........................15
Capillary connections for MIC-9 .......... 25
Caption ................................................45
Care .....................................................58
Caution...................................................8
Cell .................................................. 38,41
Cell potential ..............................39,40,43
Cell volume ..........................................66
Certificate of Conformity and System
Validation .........................................73
Changing of separating column.......... 60
charging current ..................................50
Check................................................... 11
Check marks 35
Figure............................................... 17
Column............... see Separating column
Connection.......................................18
Fix.....................................................16
Rinsing .............................................19
Column connection capillary 21
Figure .................................................6
Column holder 26
Figure .................................................6
Comment ...............................................8
Configuration in IC Net 2.1
MIC-9................................................27
Conformity............................................71
Connection
Bottle rack (6.5324.000) ..................15
Flowcell ............................................17
Injection valve ..................................16
MIC-8................................................20
MIC-8 + sample changer ................22
MIC-9................................................24
Pulsation absorber 30 .....................15
Sample Changer..............................22
Two injection valves .........................26
Waste tubing ....................................18
Connection capillary 28/29
Figure .................................................6
Pulsation absorber connection........15
Connection capillary 34
Figure .................................................6
Connections
Practical notes .................................57
Connector 27
Connect electrode cable .................18
Contaminated valves ...........................56
Control..................................................38
<Copy to clipboard>............................45
Coupling (6.2620.060)
Rinsing tubing ..................................19
current ..................................................47
current flow...........................................48
Cycle potentials ....................................42
D
Data source............................... 21,29,30
DC ........................................................37
DC mode..............................................47
Dead volume........................................62
Declaration of Conformity ....................72
Degassing of eluents ...........................57
<Delete>..............................................45
Diamond paste (6.2802.110)...............59
Disposal .................................................9
Door 1
Figure .................................................2
Double
peaks......................................62
Drain opening for spilled liquid
Precautionary rules ............................9
Drift.......................................................61
dummy cell (6.2813.030) .....................63
dummy connection ..............................30
E
E1, E2, E3.........................................41,43
Earthing ..................................................9
Electric valve 9
Figure ................................................ 4
Electrical connections
MIC-8............................................... 20
MIC-9............................................... 24
Electrical safety ..................................... 9
Electrochemical reactions................... 48
Electrode cable (6.2156.000)
Connection ...................................... 18
Electrode cable (black) 24
Figure ................................................ 6
Electrode cable (blue) 20
Figure ................................................ 6
Electrode cable (red) 19
Figure ................................................ 6
electrode surface ................................ 49
Electromagnetic compatibility............. 68
Eluent change ..................................... 57
Eluent inlet 41 of flow cell
Figure .............................................. 17
Eluent inlet 46
Figure .............................................. 16
Eluent inlet 52 Valve A
Figure .............................................. 26
Eluent inlet 58 Valve B
Figure .............................................. 26
Eluent outlet 37 of flow cell
Figure .............................................. 17
Eluent outlet 51 Valve A
Figure .............................................. 26
Eluent outlet 57 Valve B
Figure .............................................. 26
Eluent outlet connection 45
Figure .............................................. 16
Eluents................................................. 57
EMC..................................................... 68
Emission.............................................. 68
ENABLED ............................................. 45
EU Declaration of Conformity ............. 72
Evaporation ......................................... 57
F
Faults.............................................. 55,61
Feed through 2/3
Figure ................................................ 2
Filter..................................................... 40
Filter unit PEEK
Information ...................................... 55
Flow cell 23
Connection ...................................... 17
Dry ................................................... 35
Figure ................................................ 6
Mounting ......................................... 18
Technical data................................. 66
Frequency ........................................... 66
Front ...................................................... 2
Full scale.................................... 39,42,44
Fuse..................................................... 66
Fuse holder 16
Figure ........................................... 4,13
Fuses................................................... 13
817 Bioscan
75
6 Appendix
G
General information
on maintenance...............................58
General precautionary rules ..................9
GLP ...................................................... 64
H
Handling of solvents .............................. 9
Handling the 817 Bioscan ................... 35
Hazard ...................................................8
Housing................................................68
Hydrodynamic voltammogram.......51,53
I
IC column 25
Figure.................................................6
IC Net 2.1 ............................................. 36
817 Bioscan icon ............................. 36
817 Bioscan window .......................37
Configuration of MIC-9 ....................27
DC mode ..........................................39
Links................................................. 46
Manual..............................................37
Manual control ................................. 33
Method parameters ..........................39
Program............................................45
Program instructions .......................46
Pulse mode ......................................41
Scan mode .......................................43
Scan mode - Operations................... 44
Scan mode - Parameters ..................43
Settings for MIC-8............................21
Time program for 766 / 788........23,31
Time program for 813...................... 23
IC Net 2.1 Icons
817 Bioscan.....................................36
IC Separating column 25
Mounting..........................................16
Immunity ..............................................68
Information about the
Instructions for Use............................7
Injection valve
Connection ......................................16
Injection Valve A
Connections.....................................26
Injection Valve B
Connections.....................................26
Installation............................................11
Instructions for Use 8.817.1003 ............7
Instrument description...........................1
Instrument test with the dummy cell....63
Interference..........................................50
Interior .................................................... 5
Introduction............................................ 1
Ion chromatography ............................ 55
K
KELF pressure screw (6.2744.130)..... 17
L
Leaks.................................................9,61
Links..................................................... 46
Location ...............................................12
M
Mains cable
Connection.......................................14
Mains connection.................................14
Safety notes .......................................9
Technical data..................................66
Mains connection plug 17
Figure ............................................4,13
Mains switch 18
Figure ............................................4,13
On/off switching of the
instruments ......................................14
Mains voltage
Setting ..............................................12
Maintenance ...................................55,58
Malfunctions.........................................61
Manual control .....................................33
Manual valve 9
Figure .................................................4
Measuring cell......................see Flowcell
Measuring cell holder 22
Figure .................................................6
Measuring conditions ..........................48
measuring cycle...................................50
Measuring frequency ...........................50
Measuring interval................................50
Measuring potential ........................50,53
Optimization.....................................51
Measuring time ts ................................49
Method ...................................... 21,29,30
Method data.......................... 39,41,43,45
Metrohm-Service..................................58
MIC-8
IC Net 2.1 - system configuration....21
Installation ........................................20
Overview ..........................................11
MIC-9
IC Net 2.1 - System configuration ...27
Installation ........................................24
Overview ..........................................11
Microfiltration............................. 55,56,57
Mode.....................................................37
Model plate 10
Figure .................................................4
Modular IC system
Installation ........................................11
Monograph
"Ion chromatography" ........................7
"Practical Ion Chromatography".........7
Mounting screw 4
Figure .................................................4
Mounting screws 36 of flow cell
Figure ...............................................17
Mounting the column ...........................16
N
Notation..................................................8
Notes....................................................55
O
Offset ......................................... 40,42,44
On/off switching of the instruments.....14
Operating mode..............................33,65
Operation .............................................35
Operation using «IC Net 2.1» ...............36
Optimization of the
measuring potential .........................51
Optimization of the PAD parameters .. 49 Outlet 13 for spilled liquid
Figure ................................................ 4
Precautionary rules ........................... 9
Oven................................. 38,39,41,43,66
Oven 32
Figure ................................................ 6
Oven heating fan 33
Figure ................................................ 6
Oxide formation................................... 50
P
Packaging ........................................... 11
PAD - Pulsed amperometric
detection.......................................... 49
PAD parameters
Optimization .................................... 49
Parameters for the pulse mode .......... 34
Parts
Standard equipment ....................... 69
Parts and controls ................................. 2
Peak broadening................................. 62
pH.............................................. 35,48,57
Pictograms ............................................ 8
Polishing disk (6.2802.100)................. 59
Polishing the working electrode.......... 59
Potentials............................................. 49
Power consumption ............................ 66
Practical notes..................................... 55
Precautionary rules................................ 9
Precipitates..................................... 56,57
Preheating capillary 31
Figure ................................................ 6
Mounting ......................................... 16
Preparing the 817 Bioscan.................. 32
Pressure drop...................................... 62
Pressure rise........................................ 62
Pressure screw (6.2744.130)
Mounting ......................................... 16
Program instructions ........................... 46
Protection class................................... 14
Protective earth ................................... 14
Pulsation.............................................. 35
Pulsation absorber 30
Connection ...................................... 15
Figure ................................................ 6
Practical Notes ................................ 56
Pulsation Absorber (6.2620.150) ........ 35
Pulsations ............................................ 61
Pulse.................................................... 37
pulse frequency................................... 50
Pulse mode ......................................... 47
Parameters ...................................... 34
Pulsed amperometric detection
(PAD) ............................................... 49
Pump ........................... see 709 IC Pump
R
Range ........................................ 39,41,43
Reaction products............................... 49
Reactions............................................. 48
Rear ....................................................... 4
Rear panel 5/6
Figure ................................................ 5
Rectification of malfunctions ............... 61
Recycling........................................ 57,58
76
817 Bioscan
6.4 Index
Reference electrode connection 40
Figure............................................... 17
Regeneration interval........................... 50
Regeneration of separating column....56
Remote cable (6.2141.140)
Connection of sample changer...........22
Remote line connections 12/15
Figure.................................................5
Remote lines ........................................ 66
Resolution ............................................ 62
Return ..................................................71
Rinse with dist. H2O ............................19
Rinse with eluent.................................. 19
Rinsing
Column ............................................19
Tubing..............................................19
Rinsing of IC system............................ 58
Rinsing the polishing disk....................59
RS232 interface 14
Figure.................................................4
Technical data .................................66
S
Safety specifications............................ 68
Sample changer
Connection to MIC-8 .......................22
Sample inlet 49 Valve A
Figure............................................... 26
Sample inlet 55 Valve B
Figure............................................... 26
Sample loop connection 44/47
Figure............................................... 16
Sample loop connection 50/53
Valve A
Figure............................................... 26
Sample loop connection 56/59
Valve B
Figure............................................... 26
Sample outlet 48 Valve A
Figure............................................... 26
Sample outlet 54 Valve B
Figure............................................... 26
Sample time..........................................41
sampling frequency ............................. 50
Scan .....................................................37
Scan cycle ............................................43
Scan mode...........................................47
Scan rate...............................................43
Scan voltammogram ......................52,53
Screws 36
Check ...............................................17
Selectivity ........................................51,53
Sensitivity ........................................51,53
Sensitivity decreasing ..........................61
Separating column
Protection .........................................55
Separating column
Changing .........................................60
Mounting ..........................................16
Practical notes .................................55
Regeneration....................................56
Separation efficiency .......................55
Storage.............................................55
Separation efficiency............................55
Service.............................................58,64
Servicing...............................................58
Setting up the instrument.....................11
Settings
Mains voltage...................................12
Settings in «IC Net 2.1»
MIC-8................................................21
Shutdown .............................................58
Signal "overload" ..................................62
signal/noise ratio..................................51
SOP ......................................................64
Spacer..................................................59
Spilled chemicals .................................58
Splitting ................................................62
Stacked recorder icons.........................30
Standard chromatogram .....................55
Standard equipment ............................69
Standard operating procedures ..........64
Start pump ...........................................32
<Start> ................................................45
State .....................................................45
Static charges ........................................9
Stirring of the eluent .............................57
<Stop>.................................................45
Sunlight ................................................12
Syringe tubing connection 42
Figure ...............................................16
System for sugar analysis – MIC-8......20
System for the analysis of anions
and sugars – MIC-9......................... 24
System overview MIC-9....................... 29
System switch-on ................................ 32
T
t1 ......................................................... 41
t2 ......................................................... 41
t3 ......................................................... 41
Technical data..................................... 65
temperature......................................... 35
Temperature ........................................ 48
time interval
t1...................................................... 49
t2...................................................... 49
t3...................................................... 49
Time program for 766 / 788 ...........23,31
Time program for 817 ......................... 23
Transport ............................................. 11
transport damage................................ 71
Treatment of eluents ........................... 57
Tubing
Rinsing............................................. 19
V
Validation............................................. 64
Valve ............................................... 38,46
<Verify> .............................................. 45
Voltage
Technical data................................. 66
Voltammogram.................................... 51
W
Warning ............................................ 8,38
Warranty .............................................. 71
Waste container
Connection ...................................... 18
Waste tubing ....................................... 18
Working electrode
Cleaning .......................................... 59
Working electrode connection 38
Figure .............................................. 17
817 Bioscan
77
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