Antec Scientific DECADE II 171 User manual

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Antec Scientific
Industrieweg 12
2382 NV Zoeterwoude
The Netherlands
DECADE II
Electrochemical Detector
User manual
171.0011, Edition 12, 2015

Copyright ©2015, Antec, The Netherlands. 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.
ROXY, ALEXYS, DECADE, DECADE II, INTRO, Flexcell, ReactorCell, SenCell, VT-03, µ-PrepCell, SynthesisCell, ISAAC,
HyREF are trademarks of Antec. Whatman™ (word and device) and Whatrnan™ (word only) are trademarks of Whatman
lnternational Ltd. SOLVENT IFD™ and AQUEOUS IFD™ are trademarks of Arbor Technologies, Inc. Clarity®, DataApex® are
trademarks of DataApex Ltd. Microsoft® and Windows™ are trademarks of Microsoft Corporation. Excel is a registered
trademark of the Microsoft Corporation.
The software and the information provided herein is believed to be reliable. Antec shall not be liable for errors contained herein
or for incidental or consequential damages in connection with the furnishing, performance, or use of software or this manual.
All use of the software shall be entirely at the user’s own risk.

Chapter 1 DECADE II electrochemical detector 3
Declaration of conformity
We Antec Leyden B.V., Zoeterwoude, The Netherlands, declare that the
product
DECADE II™Electrochemical Detector type 171
to which this declaration relates, is in conformity with the following directives:
Safety (2006/42/EC)
Safety requirements for laboratory equipment
(Class I, Installation cat. II, Pollution degree 2)
IEC61010-1:2001 2nd ed.
Particular requirements for laboratory
equipment for the heating of materials
IEC61010-2-010:2003 2nd ed.
Immunity (2004/108/EC)
Electromagnetic immunity
EN61326-1:2006
EN61000-4-2, EN61000-4-3, ENV50204,
EN61000-4-4, EN61000-4-5, EN61000-4-6,
EN61000-4-8, EN61000-4-11
Emissions (2004/108/EC)
Electromagnetic emission
EN61326-1:2006
EN55011 (Class B), EN61000-3-2,
EN61000-3-3
Attention
Onlyuse manufacturer-supplied cable(s) to connect with other devices. Part
numbers 250.0122 (RS232 cable), 250.0130 (I/O cable) and 250.0128
(output cable). Thoroughlyconnect shielding to common. Manufacturer will
not accept anyliability for damage, direct or indirect, caused by connecting
this instrument to devices which do not meet relevant safety standards.
February 6, 2019

4DECADE II user manual, ed. 11
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
The DECADE II is ROHS compliant and in conformity with Directive
2002/95/EC Restricted use of Hazardous Substances in electrical and
electronic Equipment (ROHS).

Chapter 1 DECADE II electrochemical detector 5
Symbols
The following symbol are used on the rear panel and oven compartment of
the DECADE II:
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)

6DECADE II user manual, ed. 11
Safety practices
The following safetypractices 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 instrumentfrom 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.
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
USE ONLY WITH 250 V FUSES
EMPLOYER UNIQUEMENT
AVEC DES FUSIBLES DE 250V

Chapter 1 DECADE II electrochemical detector 7
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 byqualified service personnel. Dispose the battery
according to chemical waste only.
LC equipments should be used by trained laboratory personnel only.
Use proper eye and skin protection when working with solvents.
Additional safety requirements or protection may be necessary
depending on the chemicals used in combination with this equipment.
Make sure that you understand the hazards associated with the
chemicals used and take appropriate measures with regards to safety
and protection.
Use of this product outside the scope of this guide may present
a hazard and can lead to personal injury
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.

8DECADE II user manual, ed. 11
Table of contents
Declaration of conformity 3
Intended use 4
WEEE directive 4
ROHS directive 4
Symbols 5
Safety practices 6
Spare parts and service availability 7
DECADE II electrochemical detector 11
Installation guide 13
Unpacking 13
Installation 13
Maintenance 17
DECADE II controller 19
Introduction 19
Overview of DECADE II screens 20
Parameters 24
ALEXYS®DECADE II driver 30
Detection and parameters 33
Introduction 33
Internal organisation 33
Dual flow cell control 33
Serial mode detection 34
Parallel mode detection 34
Navigation in dual cell menu 35
Parameters 36
Range 36
Offset 37
Polarity 38
Filter 38
Noise suppression: ADF™ 39
Introduction 39
Frequency 39
Frequency of signal and noise 40

Chapter 1 DECADE II electrochemical detector 9
Low pass noise filters 42
Amplitude response plot 43
Applying ADF in chromatography 45
Events and time files 49
Introduction 49
Step by step example 49
Output events 51
Pulsed amperometric detection 55
Introduction 55
Pulse vs. DC 56
Pulse settings 57
Optimisation of wave forms 57
Output frequency 59
Peak width and integrator frequency 59
Working electrode material 60
References 62
Optimisation of working potential 63
Introduction 63
Electrochemical reactions 63
Hydrodynamic and scanning voltammogram 64
Optimisation using a voltammogram 65
Construction of a hydrodynamic voltammogram 68
Construction of a scanning voltammogram 68
Using scan mode in ALEXYS data system 70
Specifications DECADE II 73
General specifications 73
DC mode 73
PULSE mode 74
SCAN mode 74
Events 74
Rear panel I/O connections 74
Physical specifications 74
Flow cells 74
Error messages 75
Rear panel 77
Connectors A, B and C 77

10 DECADE II user manual, ed. 11
RS232C 77
Troubleshooting guide 79
No detector response 79
High cell current 79
Noisy baseline 79
Decreased sensitivity (low S/N ratio) 80
Base line oscillations 80
Saturation of output 80
Dummy cell 81
External dummy cell 81
Internal dummy cell 82
Detector accessories 83
Index 84

Chapter 1 DECADE II electrochemical detector 11
C H A P T E R 1
DECADE II electrochemical detector
Congratulations on your purchase of the DECADE II. This detector enables
you to perform all applications using electrochemical detection. The DECADE
II 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 extremelysensitive EC analyses.
The DECADE II 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 parameters can be controlled by either relays or TTL.

12 DECADE II user manual, ed. 11

CHAPTER 2 Installation guide 13
C H A P T E R 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 maybe 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 thoroughly inspected and tested to
meet the highest possible demands. The results of all tests are included.
Installation
To unpack the DECADE II, lift it from its box by both hands (Fig. 1). Never lift
the DECADE II at its front door, but at its sides.
Fig. 1. Lift instructions DECADE II.
Install the detector in an area which meets the environmental conditions
listed below:

14 DECADE II user manual, ed. 11
Table I. Environmental conditions
Parameter
Requirement
Storage temperature
-40 –50 oC (-104 –122oF)
Storage humidity
0 –90%, non-condensing
Operating temperature
4 –40 oC (39 –104 oF)
Operating humidity
20 –80%, non-condensing
Place the detector on a flat and smooth surface. Do not block the fan located
at the bottom of the detector (Fig. 2.). Blocking the fan will impair the cooling
capability of the power supply.
Fig. 2. Location of power supply fan DECADE II.
Inspect the detector for possible damage and make sure that all marked (and
ordered) items on the checklist are included. Switch ON the DECADE II by
the mains switch on the rear panel. Ensure that the power (on/off) switch and
power cord are always accessible.
HPLC connections
Use proper eye and skin protection when working with solvents.
The manufacturer will not accept any liability for damage, direct or indirect,
caused byconnecting this instrument to devices that do not meet the relevant
safety standards. The pump connected to the system should be specifically
designed for use in High Performance Liquid Chromatographyand capable
of delivering flow rates typically in the range between 1 μL/min up to 10
mL/min. Please carefully follow the next steps for a successful installation
and start-up.
1. The installation of the flow cell and column is shown in Fig. 3.
2. If a manual injector is applied with position sensor, the sensor cable
must be connected to ‘C’ on the rear panel to enable INJECT/LOAD
functions.
3. If an electrically actuated valve is mounted, connect the ‘digital
input/output cable’ to ‘B’ on the rear panel to enable INJECT/LOAD
functions.

CHAPTER 2 Installation guide 15
Fig. 3. Installation of the DECADE II.
4. Prior to connection of the HPLC system to the detector all metal
parts should preferablybe 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 dampener, the injector (in load and inject position) and to
waste.
5. 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 dampener (check with pH paper). Flush the system
with HPLC buffer.
If an ISAAC™reference electrode is used, make sure that the
buffer contains 2 mmole/l chloride (KCl or NaCl) ions.
6. Before connecting a new column read the manufacturer’s
instructions. Our experience is that thorough pre-conditioning of a
column is always required. Only a pre-conditioned column is
electrochemically clean. If not, the background current may be
unacceptably high and substantial fouling of the working electrode
occurs. For reversed phase columns flushing with 50% methanol in
water for 3 days at a low flow rate is highly recommended. Before
switching to mobile phase, flushing with water (10 column volumes)
is recommended to prevent precipitation of buffer salts.

16 DECADE II user manual, ed. 11
7. Passage of air bubbles through the flow cell will lead to unacceptable
noise levels and ‘spikes’. Therefore, the use of an in-line degasser is
strongly recommended. In our experience, a one-time degassing
step of the HPLC buffer is almost never sufficient.
8. If the DECADE II 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).
9. Consult your flow cell manual for installation of the flow cell. Connect
the flow cell to the corresponding cell connector in the oven
compartment. All cell connectors are marked with a label for
identification. In case of a DECADE II SCC connect the flow cell to
the cell connector on the left side marked “Cell 1”. The cell
connector inside the oven compartment is ESD sensitive. Make sure
that the flow cell is OFF when removing or connecting the cell cable.
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 outside of the flow cell is wet, particularly the part between the
auxiliary and working electrode connection
because substantial damage to the working electrode or electronics
may occur.
10. Before switching ON the flow cell, make sure that the buffer contains
sufficient electrolyte (buffer ions). A stable baseline will never be
obtained if the cell is switched ON with only water or another non-
conducting mobile phase. Also be sure that no air bubbles are
trapped in the flow cell.
11. 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 minute back
pressure which prevents air-bubble entrapment. The outlet tubing
should be under the liquid level, to avoid electrical noise induced by
‘dripping’ of mobile phase.
12. Set the cell potential (see page 63 for optimisation of the potential),
switch ON the flow cell (see page 19) and allow the system to
stabilise for approximately 30 min. A ‘good’ stabilisation curve shows
a mono-exponential decline without jumps and/or spikes.
13. Connect the data system to the output (see page 30).
Your system is now ready for use.

CHAPTER 2 Installation guide 17
The DECADE II 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.
Maintenance
Perform periodic leak checks on LC tubing and connections and check if the
drain on the bottom of the oven compartment is not blocked or closed.
Do not allow flammable and/or toxic solvents to accumulate. Follow a
regulated, approved waste disposal program. Empty and clean waste
container regularly. Never dispose of such products through the municipal
sewage system.
This instrument has a lithium battery inside. Replacement of the battery
should be performed byqualified service personnel. Dispose the battery
according to chemical waste only.
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.
Do not use any organic solvents to clean the exterior of the detector. Use a
cloth wetted with water only to clean the detector.
Remove any dust on the protective screens that cover the fans in the oven
compartment.
USE ONLY WITH 250 V FUSES
EMPLOYER UNIQUEMENT
AVEC DES FUSIBLES DE 250V

18 DECADE II user manual, ed. 11

CHAPTER 3 DECADE II controller 19
C H A P T E R 3
DECADE II controller
Introduction
The DECADE II has been designed for maximum functionalityand ease of
use. The control of ECD parameters is such that without reading this chapter,
it should be possible to operate the detector. This chapter is intended as a
reference guide in case questions arise during operation.
The information shown in the numerous screens is presented in alphabetical
order. For each item an explanation is given, together with the item’s nature
and the screen(s) of appearance. The nature of an item can be:
1. Control: parameters with a cursor box (‘’) can be attained via cursor
buttons and changed by the ‘value’ button.
2. Status: without a cursor box a parameter reflects the current status.
3. Functions: parameters in CAPITALS are commands accessible via
function buttons F1 - F5.
4. The 'Enter' button is only used to accept changes in cell potential. In the
top right corner of each screen the name of the present screen is
displayed. If available, the bottom left function button displays a previous
screen, and the bottom right one the next screen.
Fig. 4. DECADE II keyboard. The cursor is on ‘Range’ which allows changes
using the value buttons ‘+’ and ‘-’. The ‘Enter’ button is only used to confirm
changes in potential (Ec).

20 DECADE II user manual, ed. 11
Overview of DECADE II screens
Fig. 5. DC mode.
V o u t = + 0 . 0 5 7 V I c = + 2 3 . 4 5 n A D C 125
R a n g e = 5 0 n A E c = + 0 . 5 0 V R E M O T E
F i l t = . 0 0 2 H z C o m p = o f f 2 5 > 3 0 ° C
P R E V
P
C
A n t e c L e y d e n M A I N 12
D E C A D E - I I L C - E C w o r k s t a t i o n 2 . 0 0
C O N F I G D C P U L S E S C A N D I A G
R a n g e = 5 0 n A M a x C o m p = 2 . 5 µ A D C 13
E c = + 0 . 5 0 V # O f f s = + 1 0 % S E T U P
F i l t = . 0 0 2 H z
P R E V P O L A R = + E V E N T S N E X T
V o u t = + 0 . 0 5 7 V I c = + 2 3 . 4 5 n A D C 15
R a n g e = 5 0 n A E c = + 0 . 5 0 V S T A T
F i l t = . 0 0 2 H z C o m p = o f f 2 5 > 3 0 ° C 2 1 1 . 2 0
P R E V C E L L = O N M A R K A Z E R O N E X T
if ID > 1
1D I c = + 2 3 . 4 5 n A 4P I c = + 1 . 5 0 m A S T A T 91
2P I c = + 1 2 0 . 6 n A 5S I c = + 6 . 7 9 n A
3D I c = + 2 . 6 6 5 n A C o m p = o f f 2 5 > 3 0 ° C
P R E V M A R K A Z E R O I N J = L
V o u t = + 0 . 0 5 7 V E V E N T S 7
Fil e = 1 T e m p = 3 0 ° C S E T U P
C y c l e s = 8 9 9
P R E V R U N N E X T
V o u t = + 0 . 0 5 7 V I c = + 2 3 . 4 5 n A R U N 13
R a n g e = 1 0 n A O f f s = + 1 0 % E c = + 0 . 8 0 V
F i l t = . 0 0 2 H z C y c = 1 2 8 > 3 0 ° C w a i t i n g
Q U I T S T A R T A Z E R O
T i m e = 1 1 2 3 3 i d = 0 0 0 0 1 P R O G 8
R a n g e = 5 0 n A E c = + 0 . 8 0 V A z e r o = N O T 4 9
F i l t = . 0 0 2 H z O u t p = 0 1 1 0 O f f s = + 1 0 %
P R E V A D D D E L S C R O L L E N D C Y C L E