Antec Scientific SenCell User manual

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SenCellTM
Electrochemical Flow cell
User manual
116.0010, Edition 1, 2012
Antec Scientific
Industrieweg 12
2382 NV Zoeterwoude
The Netherlands

Copyright ©2012, 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, ISAAC, HyREF, SenCell aretrademarks 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. All othertrademarks arethe
property of their respective owners.
Thesoftware and the information provided herein is believed to be reliable. Antec shall not be liablefor errors contained herein or for
incidental or consequential damages in connection with the furnishing,performance, or use of software orthis manual. All use of the
software shall be entirely at the user’s own risk.

INTRODUCTION Table of contents 3
Symbols
The following symbols are used in this guide:
The warning sign denotes a hazard. It calls attention to a
procedure or practice which, if not adhered to, could result
in severe injuryor damage or destruction of parts or all of
the equipment. Do not proceed beyond a warning sign until
the indicated conditions are fully understood and met.
The attention sign signals relevant information. Read this
information, as it might be helpful.
The note sign signals additional information. It provides
advice or a suggestion that may support you in using the
equipment.
Intended use
This hardware should be used by trained laboratory personnel only
with a completed degree as chemical laboratory technician or
comparible vocational training. The operator should have fundamental
knowledge of liquid chromatography.
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.

4SenCell flow cell user manual, ed. 1
(U) HPLC: (Ultra) High Performance Liquid Chromatography (HPLC) is a
method for separating substance mixtures, determining substances and
measuring their concentration. This device is suitable for high-performance
liquid chromatography. It is suitable for laboratoryuse, for analyzing
substance mixtures that can be dissolved in a solvent or solvent mixture.
Check intended use: Only use the device for applications that fall within the
scope of the specified intended use. Else the protective and safety
equipment of the device could fail.
Laboratory use:
•Biochemistry/bioanalytical analyses
•Chiral analyses
•Food analyses
•Pharmaceutical analyses
•Environmental analyses
•Clinical analyses (research purpose only)
With respect to clinical analyses the device is intended for research purposes
only. While clinical applications may be shown, this device is not tested by
the manufacturer to comply with the In Vitro Diagnostics Directive.
Laboratory regulations
Observe national and international regulations pertaining to laboratory work!
For example:
•Good LaboratoryPractice (GLP) of the American Food & Drug
Administration
•For development of methods and validation of devices:
•Protocol for the Adoption of Analytical Methods in the
•Clinical ChemistryLaboratory, American Journal of Medical
Technology, 44, 1, pages 30–37 (1978)
•Accident prevention regulations published bythe accident insurance
companies for laboratory work

INTRODUCTION Table of contents 5
Solvents
Organic solvents are highly flammable. Since capillaries can detach from
their screw fittings and allow solvent to escape, it is prohibited to have any
open flames near the analytical system!
Regularly check for leaks and clogged LC tubing and connections. Test back
pressure without column. Do not close or block drains or outlets. 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.
Toxicity: Organic solvents are toxic above a certain concentration.
Ensure that work areas are always well-ventilated! Wear protective
gloves, safety glasses and other relevant protective clothing when
working on the device!

6SenCell flow cell user manual, ed. 1

INTRODUCTION Table of contents 7
Table of contents
I N T R O D U C T I O N
Symbols 3
Intended use 3
Laboratory regulations 4
Solvents 5
Table of contents 7
The electrochemical flow cell 9
Introduction 9
Three-electrode configuration 10
Working electrode 11
Detection limit 12
Cell working volume adjustment 13
Reference electrodes 18
ISAAC reference electrode 18
Salt bridge Ag/AgCl reference electrode 20
HyREF reference electrode 20
Installation 22
Introduction 22
Adjusting the SenCell working volume 23
Installation in LC system 24
Maintenance 28
Assembling/Disassembling the Cell 28
HyREF 30
ISAAC 30
Polishing 30
Coating with ISAAC solution 31
Ag/AgCl salt bridge 32
Saturation and air bubbles 32
Material 33
Procedure 33
Maintenance of the cotton wool frit 34
Working electrode 35
Polishing 35
Specifications 38
Part list 40
Index 42

8SenCell flow cell user manual, ed. 1

CHAPTER 1 The electrochemical flow cell 9
C H A P T E R 1
The electrochemical flow cell
Introduction
Congratulations on your purchase of the SenCellTM, a new electrochemical
flowcell for (U)HPLC with ECD. The SenCell has several unique features
(Patent Pending) like a stepless adjustable working volume (spacerless
concept) and toolless assembly.
The SenCell is available with a glassy carbon working electrode (WE). The
SenCell design eliminates the use of plastic/metal spacers. The working
volume of the electrochemical cell can be stepless adjusted without opening
the cell bymeans of a special key, allowing easy optimization of the detection
sensitivity for anyLC application. The working volume can be adjusted
between roughly 0 –300 nL (based on a 2 mm diameter WE). As a standard,
the salt bridge Ag/AgCl reference electrode is advised. For special
applications the HyREF™reference electrode is available. A third reference
electrode is the in situ Ag/AgCl (ISAAC™).
Fig. 1. Left side: assembled SenCell electrochemical flow cell with ISAAC
inlet block (green). The upper part, the inlet block, is separated from the
working electrode block. Right side: SenCell WE block. .
The SenCell has been developed for ultra-trace analysis in standard,
microbore and capillaryLC-EC. After extensive testing it was established that
the confined wall-jet configuration gave the very best results. In addition it
was found that the electrode materials qualityand the finishing of the
electrodes in the flow cell are decisive factors for the performance of an EC
detector.While competitive designs usually deteriorate when in use, this flow

10 SenCell flow cell user manual, ed. 1
cell, by design, improves in performance. The flow cell permit unusuallyshort
stabilisation times: trace analysis within a few hours after starting up may be
expected.
Three-electrode configuration
In the SenCell flow cell a three-electrode configuration is used (Fig. 2). The
working potential is set between the working electrode (WE) and the auxiliary
electrode (AUX). The AUX is kept at a preciselydefined reference electrode
(REF) potential by means of the so-called voltage clamp. This is an electronic
feedback circuit that compensates for polarisation effects at the electrodes.
At the WE, which is kept at virtual ground, the electrochemical reaction takes
place, i.e. electrons are transferred at theWE. This results in an electrical
current to the I/E converter, which is a special type of operational amplifier.
The output voltage can be measured by an integrator or recorder.
Fig. 2. Schematic representation of an electrochemical cell with a three-
electrode configuration.
Essentially, for the oxidation or reduction reaction it would be sufficient to use
only two electrodes. However, the three-electrode configuration has several
advantages over a two-electrode configuration. If the working potential would
be applied only over an AUX versus the WE (without REF), the working
potential would continuously change due to polarisation effects at the
electrodes, resulting in highly unstable working conditions.