Antec Scientific DECADE II SDC 174 User manual

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Antec Scientific
Industrieweg 12
2382 NV Zoeterwoude
The Netherlands
DECADE II SDC
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 SDC 3
Declaration of conformity
We Antec Leyden B.V., Zoeterwoude, The Netherlands, declare that the
product
DECADE II SDC ™ Electrochemical Detector type 174
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
Only use 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). Thoroughly connect shielding to common. Manufacturer will
not accept anyliabilityfor damage, direct or indirect, caused byconnecting
this instrument to devices which do not meet relevant safetystandards.
February 6, 2019

4DECADE II SDC user manual, ed. 3.
Intended use
For research purposes only. While clinical applications maybe shown, this
instrument is not tested by the manufacturer to complywith 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).
Antec Leyden is an ISO 9001:2008 certified company.

Chapter 1 DECADE II SDC 5
Symbols
The following symbol are used on the rear panel and oven compartment of
the DECADE II:
Consult the manual for further safetyinstructions
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 SDC user manual, ed. 3.
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
AVEC 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

Chapter 1 DECADE II SDC 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 varietyof services to support her customers after
warrantyexpiration. 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 SDC user manual, ed. 3.

Chapter 1 DECADE II SDC 9
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 availability7
DECADE II SDC 11
Installation guide 13
Unpacking 13
Installation 13
Maintenance 17
ALEXYS®DECADE II SDC driver 18
DECADE II Dialogue for SDC 19
Detection and parameters 21
Introduction 21
Internal organisation 21
Parameters 22
Range 22
Offset 23
Polarity 23
Filter 23
Noise suppression: ADF™ 25
Introduction 25
Frequency 25
Frequency of signal and noise 26
Low pass noise filters 28
Amplitude response plot 29
Applying ADF in chromatography31
Events and time files 33
Introduction 33
Output events 33

10 DECADE II SDC user manual, ed. 3.
Optimisation of working potential 35
Introduction 35
Electrochemical reactions 35
Hydrodynamic voltammogram 36
Optimisation using a voltammogram 37
Construction of a hydrodynamic voltammogram 39
Specifications DECADE II SDC 41
General specifications 41
Physical specifications 42
Error messages 43
Rear panel 44
Connectors A, B and C 44
RS232C 44
Troubleshooting guide 45
No detector response 45
High cell current 45
Noisy baseline 45
Decreased sensitivity (low S/N ratio) 46
Base line oscillations 46
Saturation of output 46
Dummy cell 47
External dummy cell 47
Detector accessories 48

Chapter 1 DECADE II SDC 11
C H A P T E R 1
DECADE II SDC
Congratulations on your purchase of the DECADE II SDC. This detector
enables you to perform all applications using electrochemical detection in the
DC mode. The DECADE II SDC 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.
The DECADE II SDC is operated by PC control software using Antec Leyden
data acquisition software or DECADE II Dialogue™.

12 DECADE II SDC user manual, ed. 3.

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

14 DECADE II SDC user manual, ed. 3.
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.
Switch ON the DECADE II SDC by the mains switch on the rear panel.
Ensure that the power (on/off) switch and power cord are always accessible.
Do not block the fan located on the rear panel. Blocking the fan will
impair the cooling capability of the power supply.
HPLC connections
Use proper eye and skin protection when working with solvents.
The manufacturer will not accept anyliabilityfor damage, direct or indirect,
caused by connecting this instrument to devices that do not meet the relevant
EMC & safetystandards. The pump connected to the system should be
specificallydesigned for use in High Performance Liquid Chromatography
and capable of delivering flow rates typically in the range between 1 μL/min

CHAPTER 2 Installation guide 15
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 electricallyactuated valve is mounted, connect the ‘digital
input/output cable’ to ‘B’ on the rear panel to enable INJECT/LOAD
functions.
Fig. 3. Installation of the DECADE II SDC.
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

16 DECADE II SDC user manual, ed. 3.
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. Onlya pre-conditioned column is
electrochemicallyclean. If not, the background current maybe
unacceptablyhigh 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.
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 SDC 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. 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.

CHAPTER 2 Installation guide 17
12. Set the cell potential (see page 35 for optimisation of the potential),
switch ON the flow cell (see page 17) 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 18).
Your system is now readyfor use. The DECADE II SDC has been developed
for continuous operation. For maximum stability it is advised to leave the
system ON continuously. If preferred, the flow cell maybe 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.
USE ONLY WITH 250 V FUSES
EMPLOYER UNIQUEMENT
AVEC DES FUSIBLES DE 250V
Do not use any organic solvents to clean the exterior of the detector. Use a
cloth wetted with water onlyto clean the detector.
Remove anydust on the protective screens that cover the fans in the oven
compartment.

18 DECADE II SDC user manual, ed. 3.
ALEXYS®DECADE II SDC driver
Full control and data acquisition is supported in the ALEXYS data system
software. Important difference with stand-alone operation is that timed events
are not executed from time files, but from the events page in the ALEXYS
software.
DECADE II SDC time files are not supported in the ALEXYS data
system. Software. Use events page instead.
Fig. 4. DECADE II SDC driver in the ALEXYS data system software.
Parameters in blue against white background are actual settings. New
parameters on the left side (Method data) can be set by clicking the Set
button.
For detailed information please consult the ALEXYS software user manual
(p/n 185.0035).

CHAPTER 2 Installation guide 19
DECADE II Dialogue for SDC
DECADE II Dialogue for Windows is a multi-functional program to control the
DECADE II electrochemical detector. DECADE II Dialogue is a tool for:
•controlling all operational parameters of DECADE II
•creating and transmitting time files to DECADE II
•controlling DECADE II IO ports for external devices
•control of DECADE II SDC and (one) LC 100
•OQ and PQ measurements
•noise measurement
There are no tools for further data analysis, therefore DECADE II Dialogue
can not be considered as fully featured chromatographysoftware package.
DECADE II Dialogue is one software package containing functionality for all
different versions. Depending on the license dongle PQ/OQ functionality will
be unlocked. In the free version - without USB licence dongle - PQ, OQ, Start
Run/Sequence are unavailable.
Fig. 5. Screenshot of the free version (no USB dongle) in combination with a
DECADE II SDC.

20 DECADE II SDC user manual, ed. 3.
Fig. 6. DECADE II Dialogue for operational control of the DECADE II SDC
electrochemical detector.
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