Antec Leyden DECADE User manual

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Edition 9, 2007 120.0010
DECADE
Digital Electrochemical
Amperometric Detector
user manual
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1
DECLARATION OF CONFORMITY
We Antec Leyden B.V., Zoeterwoude, The Netherlands, declare that the
product
Electrochemical Detector DECADE (p.n. 120.0035)
to which this declaration relates, is in conformity with the following directives:
Safety (73/23/EEC)
Safety requirements for laboratory equipment
(Class I, Installation cat. II, Pollution degree 2) IEC 1010-1
Immunity (89/336/EEC)
Electromagnetic immunity IEC 801-2/3/4 & ENV 50140
Radio frequency current injection ENV 50141 & IEC 1000-4-6
Voltage dips and interruptions IEC 1000-4-11
Emissions (89/336/EEC)
Electromagnetic radiation EN 55022, Class B (CISPR 22)
Attention
Use shielded cable(s) to connect all I/O’s with other devices. Thoroughly
connect the shielding to common. Antec Leyden will not accept any liability for
damage, direct or indirect, caused by connecting this instrument to devices
which do not meet relevant safety standards.
February 21, 2007
IN
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2 DECADE user manual, edition 9
Intended use
For research purposes only. While clinical applications may be shown, this
instrument is not tested by the manufacturer to comply with the In Vitro
Diagnostics Directive.
WEEE directive
All equipment of Antec Leyden which are subjected to the WEEE directive
shipped after August 13, 2005 are compliant with the WEEE marking
requirements. Such products are labelled with the “crossed out wheelie”,
depicted on the left site.
The symbol on the product indicates that the product must not be
disposed as unsorted municipality waste.
Collection & recycling information
Please ship the instrument back to the manufacturer (Antec Leyden, the
Netherlands) at the end-of-life time of the product. The manufacturer
will take care of the proper disposal and recycling of the instrument at
its facilities.
Shipping address for the end-of-life products:
Antec Leyden
Industrieweg 12
2382NV Zoeterwoude
The Netherlands
In case of questions, or if further information is required about the collection &
recycling procedure, please contact your local distributor.
ROHS directive
Our instruments are currently exempt from the RoHS directive because they
fall under WEEE Annex IA categories 8 and 9, which includes medical
devices and monitoring and control instruments. Nevertheless, we have taken
steps to eliminate all restricted substances from our products.
Antec Leyden is an ISO 9001:2000 certified company.
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3
Symbols
The following symbol are used on the rear panel and oven compartment of
the DECADE:
Consult the manual for further safety instructions
Frame or chassis ground terminal
The following pictograms are used in the DECADE II manual:
Caution
Caution, risk of electric shock or other electrical hazard (high
voltage)
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4 DECADE user manual, edition 9
Safety practices
The following safety practices are intended to insure safe operation of the
equipment.
Electrical hazards
The removal of protective panels on the instrument can result in exposure to
potentially dangerous voltages. Therefore, disconnect the instrument from all
power sources before disassembly. Untrained personnel should not open the
instrument.
Replace blown fuses with fuses of proper type and rating as stipulated on the
rear panel and specified in the installation section of this manual. The fuse
holder is integrated in the mains connector. Ensure that the instrument is
never put in operation with fuses of a different type. This could cause fire.
USE ONLY WITH 250 V FUSES
EMPLOYER UNIQUEMENT
A
VEC DES FUSIBLES DE 250V
Connect the detector to a grounded AC power source, line voltage 100 – 240
VAC. The instrument should be connected to a protective earth via a ground
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5
socket. The power source should exhibit minimal power transients and
fluctuations. Replace faulty or frayed power cords.
Place the detector on a flat and smooth surface. Do not block the fan located
at the bottom of the detector. Blocking the fan will impair the cooling capability
of the power supply.
General precautions
Perform periodic leak checks on LC tubing and connections.
Do not close or block the drain.
Do not allow flammable and/or toxic solvents to accumulate. Follow a
regulated, approved waste disposal program. Never dispose of such products
through the municipal sewage system.
This instrument has a lithium battery inside. Replacement of the battery
should be performed by qualified service personnel. Dispose the battery
according to chemical waste only.
Spare parts and service availability
Manufacturer provides operational spare parts of the instrument and current
accessories for a period of five years after shipment of the final production run
of the instrument. Spare parts will be available after this five years period on
an ‘as available’ basis.
Manufacturer provides a variety of services to support her customers after
warranty expiration. Repair service can be provided on a time and material
basis. Contact your local supplier for servicing. Technical support and training
can be provided by qualified chemists on both contractual or as-needed
basis.
Copyright ©2006. All rights reserved. Contents of this publication may not be reproduced in any
form or by any means (including electronic storage and retrieval or translation into a foreign
language) without prior agreement and written consent from the copyright of the owner.
The information contained in this document is subject to change without notice. Manufacturer and
its affiliated companies shall not be liable for errors contained herein or for incidental or
consequential damages in connection with the furnishing, performance, or use of this material.
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6 DECADE user manual, edition 9
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7
Table of contents
DECLARATION OF CONFORMITY 1
Intended use 2
WEEE directive 2
ROHS directive 2
Symbols 3
Safety practices 4
General precautions 5
Spare parts and service availability 5
DECADE electrochemical detector 11
Installation guide 13
Unpacking 13
Installation 13
HPLC connections 14
The DECADE controller 19
Introduction 19
Overview of all DECADE screens 20
Parameters 22
Data acquisition 29
Introduction 29
Internal organisation 29
Integrator output 30
Recorder output 31
Integrator vs. recorder output 33
Offset 34
AUTO mode and time files 37
Introduction 37
Range programming 37
Drift monitor 38
Step by step example (DECADE = Master) 39
Hardware connections: 39
Programming the AUTO mode: 40
Important note when using the drift monitor: 42
Interrupting a time file: 42
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8 DECADE user manual, edition 9
Step by step example (DECADE = Slave) 42
Hardware connections: 42
Programming the AUTO mode: 43
Interrupting a time file: 44
Other events 45
Inject/load and inject marker 45
Hold/busy 46
Overload 46
Auto zero 46
To pos A, B 46
Cell on (off) 46
Programming output functions 46
TTL contacts 47
Pulsed amperometric detection 51
Introduction 51
Pulse settings 53
Optimisation of wave forms 54
Recorder output frequency 54
Peak width and integrator frequency 55
Working electrode material 56
References 58
Optimisation of working potential 59
Introduction 59
Electrochemical reactions 59
Hydrodynamic and scanning voltammogram 60
Optimisation using a voltammogram 62
Construction of a hydrodynamic voltammogram 64
Construction of a scanning voltammogram 64
Specifications DECADE 67
General specifications 67
DC mode 67
PULSE mode 67
SCAN mode 67
AUTO mode 68
Rear panel I/O connections 68
Physical specifications 68
Error messages 69
Dipswitch settings I/O board 69
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9
Rear panel 71
TTL inputs 71
RS232C 71
Troubleshooting guide 73
No detector response 73
High cell current 73
Noisy baseline 73
Decreased sensitivity (low S/N ratio) 73
Baseline oscillations 74
Saturation of output 74
Pulse damper 75
Dummy cell 76
Index 77
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10 DECADE user manual, edition 9
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Chapter 1 DECADE electrochemical detector 11
CHAPTER 1
DECADE electrochemical detector
Congratulations on your purchase of the DECADE. This detector enables you
to perform all applications using electrochemical detection. The DECADE
includes a highly stable Faraday-shielded oven compartment accommodating
column and flow cell. This flow cell has surprised researchers for its
unsurpassed S/N ratio and therefore you now possess the best possible
combination for extremely sensitive EC analyses. To further improve the
stability of the DECADE an (electrically actuated, option) injector and a high
efficiency pulse damper can be incorporated in the oven compartment.
The DECADE covers the DC, pulse and scan mode. Important parameters in
the DC and pulse mode can be changed on a time base by user-defined
commands, which enables maximum control to fully automate the detection.
In addition, crucial settings (start, stop, hold, auto zero, cell on/off) can be
controlled by either relays or TTL (open collector type).
The DECADE can be controlled by a computer via the RS232C interface
connector (option). Supporting software ‘DECADE Dialogue’ can be obtained.
In this way maximum flexibility is warranted.
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12 DECADE user manual, edition 9
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CHAPTER 2 Installation guide 13
CHAPTER 2
Installation guide
Unpacking
Inspect the transport box for possible damage as it arrives. Immediately
inform the transport company in case of damage, otherwise she may not
accept any responsibility. Keep the transport box as it is designed for
optimum protection during transport and it may be needed again. Carefully
unpack the system and inspect it for completeness and for possible damage.
Contact your supplier in case of damage or if not all marked items on the
checklist are included.
Prior to shipment, your detector has been inspected and tested to ensure the
best possible performance. The results of the electronic tests are included in
the shipkit.
Installation
Please follow the next steps for a successful installation and start-up.
1. To unpack the DECADE, lift it from its transport box by both hands as
indicated in Fig. 1A. In any other situation the DECADE should be lifted
by both hands under the unit as indicated in Fig. 1B.
Fig. 1. Lift instructions DECADE.
2. Inspect the system for possible damage and make sure that all marked
items on the checklist are included.
3. Check whether the voltage selector is in the correct position i.e. identical
with the voltage of your local power supply. If the triangle with the voltage
range is pointing towards the small white block, the system is set to that
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14 DECADE user manual, edition 9
line voltage. If not correct, this insert has to be reversed. Use only a
supply appliance with protective grounding. The fuses are included in the
line connector.
The correct values are given on the rear panel for the different line
sources.
For 110 V (AC) ± 10%, use two 3.2 AT fuses (slow, ¼” x 1¼ ”, UL/CSA).
For 220 V (AC) ± 10%, use two 1.6 AT-fuses (slow, 5 x 20 mm, IEC127).
4. Switch ‘on’ the DECADE by the mains switch on the rear panel.
HPLC connections
Use proper eye and skin protection when working with solvents.
The installation of the flow cell, column and the injection valve (option) and
pulse damper (option) is schematically shown in Fig. 2.
5. If ordered, install the pulse damper. Connect the mounting plate with the
four bolts supplied to the pulse damper and mount the pulse damper with
four bolts. For detailed instructions on the pulse damper see page 75.
6. If ordered, the Antec supplied injection valve is equipped with a Vespel
rotor as a standard. For use of strongly alkaline solutions (pH > 10), this
should be replaced by a Tefzel rotor. Consult your supplier for details.
7. For installation of a manual injector remove the handle assembly and
place the body in the DECADE using the 2 factory-supplied mounting
screws. Re-assemble the handle assembly using the 2 set screws.
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CHAPTER 2 Installation guide 15
Fig. 2. Installation of the DECADE.
8. If a manual injector is applied, it is only part of the Faraday shield if the
yellow wire from the cell cable is clamped on a metal part of the injector.
The other end of the yellow cable is connected to ‘SHIELD’ on the
connection plate for the flow cell cable. The sensor cable must be
connected to the phone jack (P1) to make the LOAD/INJECT output on
the rear panel functional. If no injector is mounted a plug is installed. Use
of this plug does not affect the Faraday function.
9. In case of leakage the drain ensures that the oven compartment is not
flooded. For proper function of the drain the detector must be placed
level.
10. Prior to connection of the HPLC system to the detector all metal parts
should preferably be passivated with 15% nitric acid during 20 min. Make
sure that all parts that are not acid-resistant such as: nylon inlet
filters, column and flow cell are not connected during this step. The
acid is flushed through the pump, the pump tubing, the damper, the
injector (in load and inject position) and to waste.
11. After flushing with nitric acid, the system must be thoroughly flushed with
demi water. Make sure that no traces of nitric acid are left in the tubing or
pulse damper (check with pH paper). Flush the system with HPLC buffer.
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16 DECADE user manual, edition 9
If the ISAAC reference electrode is used, add 2 mmole/l chloride ions
(e.g. KCl or NaCL) to the mobile phase. Equilibrate HPLC and continue
installation.
12. Before connecting a new column read the manufacturer’s instructions.
Pre-conditioning of the column may be necessary. A pre-conditioned
column is electrochemically clean. If not, the background current may be
unacceptably high. For reversed phase columns flushing with methanol
for 3 days at a low flow rate is recommended.
13. Passage or entrapment of air bubbles in the flow cell will lead to
unacceptable noise levels. Therefore, the use of an in-line degasser in
the LC system is recommended. In our experience, a one-time degassing
step of the HPLC buffer usually is not sufficient.
14. If the detector is used for reductive ECD (at a negative working potential)
additional steps should be taken to remove oxygen from the mobile
phase. These include degassing with Helium and the use of stainless
steel tubing (impermeable for oxygen).
15. Install the flow cell as described in the flow cell manual.
Never switch ON the flow cell when:
- the cell cable is not correctly connected
- the cell is only partly (or not at all) filled with buffer
- the cell is wet outside, particularly the part between the auxiliary and
working electrode connection
because substantial damage to the working electrode or electronics
may occur.
16. Before switching ON the flow cell, make sure that the buffer is containing
electrolyte (buffer ions). If the cell is switched ON with only water or
methanol in the mobile phase, a stable baseline will not be obtained. Also
make sure that no air bubbles are trapped in the flow cell.
17. The outlet tubing from the flow cell should lead to a reservoir that is at a
higher level than the flow cell. This ensures a small back pressure which
prevents air-bubble entrapment. The outlet tubing should be under the
liquid level, to avoid noise by dripping.
18. Set the cell potential, switch ON the flow cell (see page 19) and allow the
system to stabilise for approximately 30 min.
19. Connect the data system to the integrator or recorder output (see page
29).
Your system is now ready for use.
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CHAPTER 2 Installation guide 17
The DECADE has been developed for continuous operation. For maximum
stability it is advised to leave the system ON continuously. If preferred, the
flow cell may be switched OFF at night.
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