Amperometric CN Detector PDF

AMPEROMETRIC CN DETECTOR
User Manual
SKALAR
Amperometric CN Detector
User manual
Power supply
12 V DC
Publication No: 0101099A.US

Issue date: Januari 2012
Copyright Skalar B.V.
P.O Box 3237
4800 DE Breda
The Netherlands
Tel:
Fax:
E-mail:
Internet:
+31 (0)76 5 486 486

+31 (0)76 5 486 400
info@skalar.com
http://www.skalar.com
TABLE OF CONTENTS
1
INTRODUCTION ........................................................................... 1-1

1.1
1.2
1.3
1.4
1.5
Introduction ............................................................................... 1-1

Description of the instrument ..................................................... 1-1
Safety precautions ..................................................................... 1-2
WARRANTY REGISTRATION FORM ....................................... 1-3
CUSTOMER ACCEPTANCE FORM ......................................... 1-5
UNPACKING AND INSTALLATION...............................................2-1

2.1 Unpacking instructions .............................................................. 2-1
2.2 Location..................................................................................... 2-1
2.3 Instrument requirements ............................................................ 2-1
2.4 Installation instructions .............................................................. 2-2
2.4.1 Installation of the reference electrode.................................. 2-2
2.4.2 Electrical connections ......................................................... 2-3
2.4.3 Controller functions ............................................................. 2-4
OPERATING ................................................................................. 3-1

3.1
Startup of the CN detector ......................................................... 3-1
MAINTENANCE ............................................................................ 4-1

4.1 Polishing guidelines ................................................................... 4-1
4.2 General guidelines for polishing electrodes ............................... 4-2
4.3 Polishing the silver electrode ..................................................... 4-3
4.4 Working electrodes .................................................................... 4-4
4.4.1 Removing the sheath .......................................................... 4-5
4.4.2 Storing the reference electrodes ......................................... 4-6
4.4.3 Testing the viability of the reference electrodes ................... 4-6
4.4.4 Rotation of the reference electrodes.................................... 4-6
TROUBLESHOOTING................................................................... 5-1
5.1
Electronic troubleshooting ......................................................... 5-1
TECHNICAL INFORMATION ........................................................ 6-1

6.1
Controller functions.................................................................... 6-1
INTRODUCTION
1.1
Introduction
Chapter 1
Introduction
1-1
Amperometric detection is a highly sensitive technique. The currents

measured typically fall in nano ampere range. Hence, smooth operation
can easily be influenced by electrical disturbances in the environment. Also,
since detection is due to a chemical reaction, its response (and baseline
drift) is temperature-dependent; this is very noticeable at high detector gain.
The Amperometric CN detector consists of a Petit Ampre Amperometric
controller (range 5-200 nA/V, type LC-3D) and a thin-layer transducer cell.
Figure 1.1
1.2
Description of the instrument

A complete thin-layer transducer cell (see Figure 1.1) includes three
separate electrodes: a working electrode, a reference electrode, and an
auxiliary electrode.
The working electrode consists of a metal rod embedded in a plastic block.
Silver is used as working electrode. The block is made of PEEK (polyether
ether ketone) and is resistant to solvents and temperatures normally used
in electrochemistry. Working electrodes are maintained by polishing as
Chapter 1
Introduction
1-2
needed, using the instructions given in this manual (Chapter 4). We do not
recommend polishing methods other than those described in this manual.
The reference electrode is a silver/silver chloride. The reference electrode
is housed within the auxiliary electrode block.
The auxiliary electrode is a s tainless steel block. A gasket is sandwiched
between the auxiliary and the working electrode blocks, forming the thinlayer channel in which the electrochemical reaction takes place.
1.3
Safety precautions
Only qualified persons should carry out all adjustments, maintenance and
repair of the instrument.
1.
The detector unit is designed for laboratory use.
2.
Before the controller is connected to the mains and switched on, check
whether the required voltage (indicated on the type plate at the back of
the instrument) corresponds with the line voltage.
3.
The instrument power cord must only be plugged into a line supply
outlet with ground protector (earth). If an extension cord is used, make
sure that the protector line is not interrupted.
4.
Before any service, repair or change of parts, the instrument has to be

disconnected from all power supplies. Service and repair work on the
voltage carrying instruments should be av oided whenever possible. If
such work is absolutely necessary qualified personnel, who are aware
of the hazards, should carry it out.
5.
Whenever it is likely that safe operation is impaired, the instrument

must be made inoperative and secured against unintended operation.
The appropriate servicing personnel must then be informed.
6.
Never place the unit in an ar ea where it will be exposed to extreme

heat, moisture or corrosive materials.
7.
The controller must be disconnected from all electrical sources when a

battery is to be renewed.
Skalar B.V. does not accept liability for any consequences caused by
irresponsible use or irresponsible handling of the instrument, nor for the
effects and consequences induced by its use.
1.4
Chapter 1
Introduction
1-3
WARRANTY REGISTRATION FORM

The warranty period is 12 months and starts on the date of shipment. To
activate the warranty, please return the signed warranty registration form by
the Skalar Service Desk. The warranty registration form should be received
within 2 months from the shipment date.
Warranty is ex Skalar Analytical BV and does not include travelling,
expenses and working hours at customers location.
Warranty is subject to the following exception(s): Glassware breakage.
Consumable products, brokerage and t ransport costs for the replacement
parts replaced under the warranty are to the clients account. Skalar will not
be responsible for malfunctioning of the instrument if third party
components are used in the instrument.
All Skalar contracts are according General terms and conditions for the
Instrument branch as issued by FHI Het Instrument, which are available on
request.
REGISTRATION FOR WARRANTY:
Purchase
Serial no.:
Date of
Distributor:
Company
Address:
Post
City
Country:
Contact
Telephone
Fax
E-mail
Company
Name:
Signature:
The warranty registration form will only be valid when accompanied by the
signed customer acceptance form.
Please return this form to:
Date:
SKALAR ANALYTICAL B.V.

PO Box 3237
4800 DE Breda
The Netherlands
Attn.: Service desk
1.5
Chapter 1
Introduction
1-5
CUSTOMER ACCEPTANCE FORM
Company
Address:
Post
City:
Country:
Date:
The undersigned authorized officer confirms that the performance of the

instrument, as per the purchase order number as mentioned on t he
warranty registration form, is according to the specifications as submitted
by the manufacturer.
YES
NO
Remarks:
Signature
Name
Chapter 2
Unpacking and installation
UNPACKING AND INSTALLATION
2.1
Unpacking instructions
2-1
While unpacking do not discard any packing materials, till all parts have
been unpacked and checked against the packing list to insure all items are
accounted for. If any item is missing first check the packing. If it still cannot
be found, make a note of it giving as clear a description as possible using
part numbers from the manual and i mmediately inform the forwarder and
the supplier (see delivery conditions). Even when you think that all items
have been accounted for, check the packing.
Should there be any damaged or broken parts, repack it in the original
packing, and immediately inform the forwarder and the supplier who will
give further instructions. If the goods are supplied on trial, the original
packing material must be used for return shipment unless better is
available.
2.2
Location
The controller should only be pl aced on a l evel, clean, dry and s turdy
surface behind (if possible on a s helf) or beside the analysis system to
avoid hampering the performance by vibrations. The ambient temperature
should be between +10Cand +40C, humidity 20% to 80%, non
condensing. Avoid very dry, carpeted areas, as static electricity can affect
the performance.
Do not locate the control unit:
In direct sunlight.
Near an air conditioning unit.
Near any heat or cooling source.
Near equipment that generates intensive magnetic or electric fields.
Near equipment that generates high frequency.
The thin-layer flow-cell is placed on the analysis system (see installation

instructions).
2.3
Instrument requirements
Power supply is provided by an adapter cable that provides 12 V DC
unregulated at 10 mA. Connect only the complete system to the same
power supply to avoid spikes by other laboratory equipment. The adapter
cable must only be connected to a line supply with ground protector (earth).
If an ex tension lead is used make sure the ground protector line is not
interrupted.
Chapter 2
2-2
The controller is operated with an internal battery. The battery is a 7.2 V

100 mA/hr NiCad in a standard 9 V battery form. If the LC-3D electronics
are turned off, the battery will fully charge in 12 hours; if the unit is on, it will
take 24 hours for a full charge. With a full charge on the battery, the unit will
run 2024 hours. The POWER switch turns the electronics OFF and ON.
The modular supply is powered as long as it is plugged in.
VERY IMPORTANT!
Use only NiCad or NiMetal Hydride batteries! Use of other batteries
(alkaline or Ph acid) may cause acid leakage or explosion, and will
definitely void the warranty. Please dispose of old batteries in an
environmentally responsible manner. The unit must NEVER be operated
without the battery in place, or damage to the instrument will occur. The
battery needs to be replaced every year even if the unit is always run from
AC power.
2.4
Installation instructions
2.4.1
Installation of the reference electrode
Figure 2.1 Layout of the thin-layer cell

1.
Connect the tubing coming from the chemistry module to the In

connector and the tubing to the waste to the Out connector.
2.
Open the cover of the thin-layer cell by its thumb wheels.
3.
Start the pump on the system. The reference electrode well in the
auxiliary electrode will fill up. Siphon off this fluid several times, until
there are no air bubbles in the well.
2.4.2
Chapter 2
2-3
4.
Stop the pump. Insert the reference electrode O-ring into the well, and
push it down so it sits flush on the ledge inside the well.
5.
Siphon off excess fluid to the level of the o-ring.
6.
Take a reference electrode from its storage solution and carefully insert
the reference electrode through the o-ring, so no bubbles are trapped
under it.
7.
Dry the area on top of the o-ring, and any fluid that squirted out behind
the auxiliary electrode. Place the bushing on top of the reference
electrode, and screw down the locking collar, finger tight.
8.
Route the detector outlet to waste. Then start the pump and check for
leaks.
Electrical connections
Required components:
Cable connecting the thin-layer flow cell to the controller
Adapter Cable controller to mains
Cable controller to interface (via signal offset compensator)
Note:
Make sure that the controller is in Standby mode before a

connection is made or the controller is switched on/off.
Figure 2.2 Rear side controller

Procedure:
1.
The cell lead cable is attached to the CELL connector (see Figure
2.2).To make the connection, insert the cell lead cable connector into
this socket until the two components snap into place. Do not force this
connection; make certain the two components are properly aligned
before making the connection. The cable has three leads with color
coding for connection to the thin-layer cell. The black lead is connected
to the working electrode, the white lead to the reference electrode and
the red lead to the auxiliary electrode (see Figure 2.3).
2.
Connect the GND/IOUT banana jacks to the Input 1 connection of the

Signal Offset compensator. Connect the output of this compensator as
described in its manual.
3.
Connect the adapter cable to the POWER connector and the mains.
4.
Close the cover of the thin-layer cell.
Chapter 2
Figure 2.3 Cell connections
2-4
Amperometric CN detector
Chapter 3
OPERATING
3.1
Startup of the CN detector
Operating
3-1
Note: The CELL MODE switch should be placed in STBY before the
POWER switch is turned to ON.
1.
Make sure that the system is hooked up and running properly. There
should be no bubbles in the flow cell, and all connections are as
previously described.
2.
Adjust the baseline in FlowAccessTM with the Signal Offset

compensator.
3.
Make sure that the CELL

MODE switch is in the
STBY position.
4.
Turn the POWER switch

on
5.
Set the desired potential.

Turn the DISPLAY knob
to the APP E V position,
then turn the APP E
adjusting knob until the
correct potential (= 0 V) is
displayed.
6.
Set the appropriate filter

(= 0.08 Hz).
7.
Set the RANGE control to

its
least
sensitive
(highest) setting (= 200
nA).
8.
Set the OFFSET to a

near-zero reading by
changing the DISPLAY
knob to OFFSET and
turning
the
OFFSET
adjusting knob. Then turn
the DISPLAY knob to the
OUTPUT position.
9.
Figure 3.1
Turn the CELL MODE
switch to the CELL
position. This applies potential to (turns on) the working electrode.
10. When the electrode is first turned on, you should see a large current
signal. This is the charging and transient background current, and will
gradually decay to a steady-state background. For the application a
stabilisation time of 120 minutes is required for new electrodes and 30
minutes after day 1.
11. When the background stabilizes, turn the OFFSET adjusting knob until
the output is near zero. Then change to the desired RANGE (=50 nA)
and, if necessary, rezero with the OFFSET adjusting knob.
12. The system is now ready for standards and samples.
MAINTENANCE
4.1
Polishing guidelines
Chapter 4
Maintenance
4-1
The objective of polishing the electrode is to remove the redox reaction

products that accumulate during some experiments. The rate of electrode
coating (and corresponding decrease in responsiveness) depends on:
1.
The analyte molecule
2.
The concentration of the analyte molecule
3.
The composition of the electrolyte solution (including pH)
4.
The applied potential
5.
The frequency of use
Electrodes used in liquid chromatography may last for several months

without repolishing in some applications. LCEC has the advantage of using
a flowing stream which helps to remove redox products, and deals with
much lower concentrations of analytes than does voltammetry. Electrodes
also can accumulate material by adsorption from the atmosphere. For
example, components in cigarette smoke and aerosols of various
compositions can affect electrode performance. Silver is easily oxidized
under such conditions and should be carefully repolished to remove oxides
prior to use. There are many rumors and horror stories about electrode
polishing. There are also some home-made polishing recipes that we
specifically discourage. The use of concentrated acidisone. Use of jewelers
rouge, toothpaste, Aunt Ruths fruit cake (vintage1972) and other abrasive
compounds should be fervently avoided. Many of these home remedies do
not work and may harm the electrode. One thing is certain: The need for
polishing varies dramatically with the application.
There are many potential causes for that glitch or noise in the baseline.
Dont routinely conclude that polishing the electrode will cure all. As a rule,
polishing is justified when you see a gradual decrease in the response of
the electrode (see Figure 4.1). You can live with decreased response if you
are still able to quantitate the peaks of interest and if you periodically inject
a set of standards. In many cases, a light buffing of the working electrode
surface with a methanol-soaked lab tissue is all thats needed to restore the
electrode. Try this first! If such a treatment improves the response only
slightly, then the use of polishing abrasives is the next logical step.
Chapter 4
Maintenance
4-2
Figure 4.1 Example of gradual decrease of the working electrode

A series of one to three abrasives is used for polishing, progressing from
coarser materials to very fine polishes used on soft-surfaced pads. The
polishing process should remove a negligible amount of electrode material.
In most cases, a single abrasive is used to lightly erode the surface and
physically remove the contaminants. Precious metal electrodes or
chemically modified electrodes (e.g., gold/mercury amalgam) tend to
require a series of two or three abrasives to restore the original mirror-like
finish. All polishing steps require extensive rinsing and flushing of the
electrode before moving onto the next stage. Without this washing, minute
particles from the previous polishing step will be carried over and will hinder
the progression towards smaller-sized articles of abrasive. Plastic squeeze
bottles with thin nozzles are best for rinsing. Fill one with clean, distilled
water for rinsing alumina polish. Fill another with methanol for rinsing
diamond polishes. Label the bottles. A major concern of polishing is that
you do not erode the softer electrode below the surface of the surrounding
plastic or glass. This can be avoided by polishing the electrode on a hard
flat surface. Follow the general guidelines in Chapter 4.2 when handling
your working electrode.
4.2
General guidelines for polishing electrodes

1.
It is important to use the polishing materials provided by BAS and to

follow the recommended procedure. The polishing kit provided with
your BAS instrument gives you all materials needed for all polishing
procedures. Individual polishes, pads, or the entire kit can be
purchased separately.
2.
Before use, shake all bottles of polishing slurry well to ensure that all
the grit is evenly suspended.
3.
Only one grade of polishing slurry is to be applied to the pad; that is,
use a different pad for each polishing step. Do not add fresh polishing
compound to pads once a particular polishing step has been initiated;
add sufficient slurry at the beginning. If additional lubrication is
required, add water to the pad.
4.
While most individual nylon (white) polishing pads may be re-used, the
fine grit polishing pad (black to dark gray in color) should be used one
time only. If used more than once, excess scratching may occur due to
Chapter 4
Maintenance
4-3
the spaces between the grit being filled in with PEEK, causing a
deeper pressure scratch to occur.
5.
The diamond slurries (15-m blue,6-m orange,3-m yellow, and1-m

gray) have an oil base, so a methanol or acetone flush of the electrode
is required.
6.
The pads have self-adhesive backs and are less likely to rise off the
glass when wetted if applied to the glass plate the previous day. Clean
the glass plate with methanol first. Then peel the pad and push down
from the center out to the edge so no air pockets are trapped between
pad and plate (so no high spots are produced). Label each plate for the
appropriate grade of slurry to be used.
7.
Moisten the pads with distilled water a few minutes prior to use. This
will aid in breaking up any clumps of grit that were not rinsed off from a
previous use. The excess polishing grit should always be rinsed off the
pads after use to lessen the chances of clumping. Large clumps of grit
will excessively scratch the gold and PEEK.
8.
Rinse all surfaces of the electrode block free of any polishing

compound (grit). Since the polishing schedule progresses from coarse
to fine, it is very important not to mix large and small particle sizes.
9.
Polish the electrode on pads attached to the heavy glass plates

provided in the polishing kit. Hold the electrode surface as parallel to
the surface of the glass as possible. This is especially important with
voltammetry electrodes and will ensure that the surrounding plastic is
not worn unevenly.
10. Moving the block in a figure-eight pattern is optimal for uniform

polishing. However, an alternating clockwise/counterclockwise motion
is also acceptable. During all polishing steps, apply even pressure to
the electrode block. This may be accomplished by alternating the
position on the block to which you are applying pressure:
11. Never attempt to remove the actual electrode material from the
supporting plastic. This will destroy the electrode.
12. Do not heat the electrode when drying. Allow it to dry at room
temperature. Any heating of the electrode should be attempted with
caution due to the difference in the coefficients of expansion of the
electrode and the supporting plastic or glass.
4.3
Polishing the silver electrode

1.
Remove a new microcloth disk from the polishing kit. (Microcloth is

brown and has a soft, velvety texture.) Peel away the backing to
expose the adhesive, and attach the disk to the glass plate. Use a
permanent marker to label the glass with the type of polishing fluid
used. It is possible to re-use the disks several times, but it is important
to use the same type of polish each time. Your label will remind you
which polish you used. Now follow these steps (refer to Figure 4.2
2.
Rinse the electrode surface with water to flush away any encrusted
material on the surface. Follow this with a methanol rinse. Wipe dry
with a fresh lab tissue.
3.
Wet the disk surface with clean DISTILLED water. Shake the alumina
suspension and add several drops of alumina polish, spacing them
evenly around the pad surface.
Maintenance
4.
Place the electrode face down

on the pad. Using a smooth,
circular motion, and even
pressure, move the electrode
all over the pad. By reversing
the polishing direction and
rotating the electrode 90 at
regular intervals, you will
prevent uneven wear of the
electrode. After1 2 minutes,
remove the electrode and
rinse it well with DISTILLED
water.
5.
Electrodes may be sonicated

to remove residual abrasive
particles.
Immerse
the
electrode surface in a shallow
amount of DISTILLED water in
a beaker that has been placed
in the water of a low-power
(150 watts or less) ultrasonic
cleaner. Sonicate for no more
than 5 minutes (longer periods
may overheat and damage the
electrode). Rinse again with
distilled water from the
squeeze bottle and shake off
the remaining water.
6.
4.4
Chapter 4
4-4
Figure 4.2
Rinse the electrode briefly with methanol and wipe it dry. The electrode
is now ready to use. Do not touch the electrode surface with your
fingers, or place the surface in contact with sharp objects or other
materials which could scratch it.
Reference electrodes
The purpose of the reference electrode is to provide a stable, reproducible
voltage to which the working (detector) electrode potential may be
referenced. A reference electrode may be considered a small battery
whose voltage (potential) is determined by the chemistry taking place
between a solid conductor (usually a metal salt) and the electrolytic solution
around it. Ideally, if a small current is passed through the electrode, the
potential change is negligible, and in any case, returns to the initial value
when the current ceases. In addition, the potential value should not vary
with time and should be reproducible from electrode to electrode. The most
common reference electrodes meeting these criteria are the
mercury/mercurous chloride (calomel) and the silver/silver chloride
(Ag/AgCl) electrodes.
Each Ag/AgCl reference electrode is individually inspected and tested for
adherence to an acceptable range relative to a standard calomel electrode.
The model used is the shortest (3 cm), and fits into the thin-layer flow cell. It
features glass-body construction with a porous ceramic frit at the solution
interface. The filling solution is 3M NaCl gel that has been saturated with
AgCl; the gel is semi-solid and will appear cloudy with occasional particles.
Chapter 4
Maintenance
4-5
Use of a reference electrode with bubbles lodged in the tip may prevent
electrical contact with the sample solution and cause damage to the
working electrode. Bubbles can be dislodged by holding the top of the
electrode with one hand and tapping the electrode near the Vycor tip with
the other hand until the bubbles rise to the top.
4.4.1
Removing the sheath

Every Ag/AgCl reference electrode is shipped with a colored plastic sheath
that covers the porous tip and retards drying. Immediately upon receipt,
remove this sheath by rolling it down from the glass body to the tip
(see Figure 4.3). The plastic will roll down and slide off the end of the
electrode. Do not tug at the sheath or hold the electrode by the pin while
you are doing this. If you have trouble removing the sheath, make a small
cut at the upper edge of the sheath using small scissors, and try again.
Figure 4.3 Removing the sheath

Once the sheath is removed, store the electrode tip in 3M NaCl as
shown in Figure 4.4. The Ag/AgCl reference electrodes are easily ruined
by drying. Keep the tips wetted at all times and store in 3M NaCl when not
in use.
Figure 4.4 Storing the reference electrodes
4.4.2
Chapter 4
Maintenance
4-6
Storing the reference electrodes

Be sure that you check the electrodes periodically and replace the solution
in the storage vessel with fresh 3M NaCl to keep the tips wet. Do not
entirely immerse reference electrodes. Keep the connecting pins dry, or
they will corrode and contaminate the reference electrode.
Reference electrodes will naturally change with use due to the transport of
ions and solvent across the junction (ceramic or Vycor tip). The rate of
change is a function of the difference in composition between the sample
solution and the filling solution (3M NaCl gel). It is advisable to change to a
new reference electrode frequently, at least once per week. Storing the
reference electrode in 3M NaCl between experiments will extend its
lifetime. In spite of all attempts to extend their lifetimes, reference
electrodes are still expendable items, so be certain to have spares on hand
as needed.
4.4.3
Testing the viability of the reference electrodes

If you are concerned about the viability of a particular Ag/AgCl reference
electrode, you can test it using a simple volt meter, additional reference
electrodes of the same type (or a calomel reference electrode), and a small
beaker of 3M NaCl (see Figure 4.5). Read the potential difference between
the electrodes on the volt meter. Ideally the difference between two
electrodes of the same type would be zero. However in actual practice
there is commonly some variation.
Figure 4.5
4.4.4
Rotation of the reference electrodes

We recommend that three reference electrodes be rotated in your system.
Keep one electrode in your system for about two weeks. Turn the detector
to STANDBY before removing and replacing the electrode.(Failure to do so
can ruin a glassy carbon working electrode.) Rinse excess 3M NaCl
Chapter 4
Maintenance
4-7
storage solution off the replacement reference electrode before inserting it

into the cell. Replace the bushing and O-ring if they show signs of wear.
Turn the cell on. Place the first electrode into the storage container. In
another two weeks, replace the reference electrode with the third reference
electrode provided in the kit. By rotating the three reference electrodes
provided with your detector on a continuous basis, you can maximize their
lifetimes. Depending on the mobile phase conditions and detector use, the
reference electrodes can last from 6- 12 months. When you replace
reference electrodes, replace all three of them at the same time.
TROUBLESHOOTING
5.1
Electronic troubleshooting
Chapter 5
Troubleshooting
5-1
1.
With the CELL MODE switch in the STBY position, turn the POWER
on. The LCD display should be active. If the LCD does not come on,
check the power supply and wall outlet. If the power supply and wall
outlet are okay, replace the 7.2V NiCad battery.
2.
Set the DISPLAY switch to OFFSET nA and adjust the OFFSET

control knob to zero
3.
4.
Set the RANGE to 200 nA.

Set the FILTER to 0.3Hz.
5.
Plug the black probe of a digital volt meter into the GND, and the red
probe into the green 1V output jack. Set the CELL MODE switch to the
TEST position. Using the first two columns of Table 6.1 as a guide, set
the POTENTIAL and RANGE as indicated, and compare output of the
front panel display and the volt meter reading with the table. Using the
first entry from the table as an example, when APP E is set to 1.0 (V)
and the RANGE is 10 nA, the output as read on the front panel display
should be 10.0 nA and the corresponding output voltage should be 1 V.
6.
Check the remainder of the outputs (current and potential) for the
applied potentials and ranges in the table. It may take 10 to 15
seconds for the volt meter reading to stabilize when switching between
certain ranges, due to the influence of the filter on the controller. This is
normal.
7.
Change the display to Offset. Turn the OFFSET control knob until a
reading of 10 nA display. The output reading on the volt meter should
be 0-150 mV. Again, volt meter readings may take 10-15 seconds to
stabilize. If the instrument fails any step of this procedure, contact BASi
customer service personnel.
Expected readings for self test:

Applied E (V)
Range
Display output
Back panel output
1.000
1.000
1.000
0.100
0.100
0.100
200nA
100nA
50nA
20nA
10nA
5nA
98.0-102.0nA
98.0-102.0nA
98.0-102.0nA
9.50-10.50nA
9.50-10.50nA
9.50-10.50nA
0.490-0.510
0.980-1.020
1.960-2.040
0.475-0.525
0.950-1.050
1.900-2.510
Chapter 6
TECHNICAL INFORMATION
6.1
Controller functions
Technical information
6-1
DISPLAY
This switch selects the function to
be monitored by the internal 31/2digit LCD voltmeter. The
selections are:
APP E V displays the applied

potential in volts.+1.500 V to
1.500 V
OFFSET nA displays the

offset current in nA: +199.9
nA to 199.9 nA
OUTPUT nA displays the

output current in nA
RANGE
This switch selects one of six
possible output (gain) ranges in
nanoamps per volt:
5, 10, 20, 50, 100, 200 nA/V.
For example, a setting of 10 nA
with a cell current of 5nA would
produce an output of 0.5 V. The
output is capable of swinging +5
V to 5 V, which provides a fivetimes overrange capability at the
output jacks.
Figure 6.1
Note: If the current exceeds 500 nA on the 5, 10, or 20 nA ranges, or if the

current exceeds 5 A on the 50, 100, or 200nA ranges, potential
control may be lost. For this application the value is set at 10 nA.
CELL MODE
This switch controls the application of potential to the cell. In the STBY
mode, the working, reference, and auxiliary are disconnected from the cell.
In the CELL mode, all electrodes are connected and the selected potential
is applied. The TEST mode is used for trouble-shooting the controller for
electronic problems and connects to an internal dummy cell. The dummy
cell (10 M ohm) provides 100 nA/V applied E.
Chapter 6
Technical information
6-2
Note: The CELL MODE should always be set to STBY before handling the
cell lead connections, as static that has accumulated may discharge
into the cell lead connections, damaging your unit.
APP E
The APP E knob adjusts the applied potential. This is a 10-turn adjustment
with 1.5 V at full counterclockwise, and +1.5 V at full clockwise. The
DISPLAY switch must be set to APP E V when the APP E adjustment is
made. For this application the value is set at 0 V.
OFFSET
The OFFSET knob provides a 10-turn adjustment of offset current, to zero
output for a steady-state background current. The offset range is 199.9 nA
at full counterclockwise to +199.9 nA at full clockwise. For this application
the value is set at 10 nA.
Figure 6.2
POWER
The POWER switch turns the electronics OFF and ON. The modular supply
is powered as long as it is plugged in. The CELL MODE switch should be
placed in STBY before the POWER switch is turned to ON.
FILTER
The FILTER switch controls the filtering of the output. There are three
settings: 0.03, 0.08, and 0.3Hz. These settings correspond to the 3 dB point
of the frequency roll-off. The 0.03 Hz is the most heavily filtered output and
the 0.3Hz setting is the least filtered output. For this application the filter
is set on 0.08 Hz.

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AMPEROMETRIC CN DETECTOR

Publication No: 0101099A.US

+31 (0)76 5 486 486

INTRODUCTION ........................................................................... 1-1

Introduction ............................................................................... 1-1

UNPACKING AND INSTALLATION...............................................2-1

OPERATING ................................................................................. 3-1

Startup of the CN detector ......................................................... 3-1

MAINTENANCE ............................................................................ 4-1

Electronic troubleshooting ......................................................... 5-1

TECHNICAL INFORMATION ........................................................ 6-1

Controller functions.................................................................... 6-1

Amperometric detection is a highly sensitive technique. The currents

Description of the instrument

The detector unit is designed for laboratory use.

Before any service, repair or change of parts, the instrument has to be

Whenever it is likely that safe operation is impaired, the instrument

Never place the unit in an ar ea where it will be exposed to extreme

The controller must be disconnected from all electrical sources when a

WARRANTY REGISTRATION FORM

SKALAR ANALYTICAL B.V.

CUSTOMER ACCEPTANCE FORM

The undersigned authorized officer confirms that the performance of the

Unpacking and installation

UNPACKING AND INSTALLATION

Near an air conditioning unit.

Near any heat or cooling source.

Near equipment that generates intensive magnetic or electric fields.

Near equipment that generates high frequency.

The thin-layer flow-cell is placed on the analysis system (see installation

Unpacking and installation

The controller is operated with an internal battery. The battery is a 7.2 V

Installation of the reference electrode

Figure 2.1 Layout of the thin-layer cell

Connect the tubing coming from the chemistry module to the In

Open the cover of the thin-layer cell by its thumb wheels.

Unpacking and installation

Siphon off excess fluid to the level of the o-ring.

Cable connecting the thin-layer flow cell to the controller

Adapter Cable controller to mains

Cable controller to interface (via signal offset compensator)

Make sure that the controller is in Standby mode before a

Figure 2.2 Rear side controller

Connect the GND/IOUT banana jacks to the Input 1 connection of the

Close the cover of the thin-layer cell.

Unpacking and installation

Figure 2.3 Cell connections

Startup of the CN detector

Adjust the baseline in FlowAccessTM with the Signal Offset

Make sure that the CELL

Turn the POWER switch

Set the desired potential.

Set the appropriate filter

Set the RANGE control to

Set the OFFSET to a

The objective of polishing the electrode is to remove the redox reaction

The analyte molecule

The concentration of the analyte molecule

The composition of the electrolyte solution (including pH)

The applied potential

The frequency of use

Electrodes used in liquid chromatography may last for several months

Figure 4.1 Example of gradual decrease of the working electrode