IKA ElektraSyn 2.0 User manual

ElektraSyn 2.0

Declaration of conformity
We declare under our sole responsibility that this product corresponds to the regula-
tions 2014/35/EU, 2006/42/EC, 2014/30/EU and 2011/65/EU and conforms with the
standards or standardized documents: EN 61010-1, EN 61010-2-051, EN 61326-1,
EN 60529, EN ISO 12100.
A copy of the complete EU Declaration of Conformity can be requested at
[email protected].

4
/// DEVICE SETUP
› ElectraSyn 2.0 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
› Display . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
/// SAFETY INSTRUCTIONS
› Explication of warning symbols . . . . . . . . . . . . . . . . . . . . . 8
› General information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9
› Device design . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9
› Permissible medium / contaminants / side reactions . . . . . 10
› Experimental procedures . . . . . . . . . . . . . . . . . . . . . . . . . 10
› Accessories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
› Power supply / Switching off . . . . . . . . . . . . . . . . . . . . . . 12
› Protecting your device. . . . . . . . . . . . . . . . . . . . . . . . . . . 12
/// PROPER USAGE
› Basics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12
/// START-UP
› Your ElectraSyn package . . . . . . . . . . . . . . . . . . . . . . . . . 13

5
/// CYCLIC VOLTAMMETRY
›Scope of delivery. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
›Reference Electrode (RE) . . . . . . . . . . . . . . . . . . . . . . . . . 17
›Working Electrode (WE). . . . . . . . . . . . . . . . . . . . . . . . . . 18
›Counter Electrode (CE). . . . . . . . . . . . . . . . . . . . . . . . . . . 18
› CV setup. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19
/// WARRANTY
› Regulations. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22
/// SETTING UP A REACTION
›Basic guide . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
/// SMART ASSIST
›Take the guesswork out of Electrochemistry . . . . . . . . . . . 16
/// TECHNICAL DATA
›ElectraSyn 2.0 in detail . . . . . . . . . . . . . . . . . . . . . . . . . . 21

6 Device setup
Device setup
/// ElectraSyn 2.0
AON/OFF switch (standby)
BRotating knob (chose values / start-stop)
C"Menu" button
D"Cyclic Voltammetry" button
E"Back" button
F"Graph" button
G"Lock" button
Explication of symbols
HDisplay
IPower socket
JContact thermometer jack
KMicro USB interface
LThreaded hole for vertical rod
MSingle vial holder
JKI
H
LM
BCFGEDA

Device setup 7
/// Display
01 Set speed
02 Actual / set voltage
(depending on selected operating mode)
03 Actual / set current
(depending on selected operating mode)
04 Charge activated
05 Motor activated
06 Timer / remaining charge
07 Polarity indicator
08 Actual temperature
(in connection with an external PT1000 sensor)
Display
09
Operation mode
(constant voltage / constant current)
10 USB connection with PC
11 All operation elements locked
12 USB-stick pluged into USB interface
13 Connection with PC established
14 Wireless connection established
15 Estimated duration of experiment /
charge counter
07 08 09 10 11 12 1413
03
02
15
0105 0406

8 Safety instructions
Safety instructions
/// Explication of warning symbols
Indicates an (extremely) hazardous situation, which,
if not avoided, will result in death, serious injury.
Indicates practices which, if not avoided, can result in
equipment damage.
!
Indicates a potentially hazardous situation, which, if
not avoided, can result in death, serious injury.
Indicates a potentially hazardous situation, which, if
not avoided, can result in injury.
Attention!
- risk of damage due to magnetism.
DANGER!
- note on hazards arising from a hot surface.

Safety instructions 9
Safety instructions
/// General information
› Read the operating manual in its entirety before using
the device and follow the safety instructions.
› Keep the operating manual in a place where it
can be accessed by everyone.
› Ensure that only trained staff work with the device.
› Follow the safety instructions, guidelines, occupational
health and safety and accident prevention regulations.
/// Device design
Danger! ( )
Do not operate the device in explosive atmosphere and with hazardous
substances.
› Set up the device in a spacious area on an even, stable,
clean, non-slip, dry and fireproof surface.
› The feet of the device must be clean and undamaged.
› Check the device and accessories for damage before each use.
Do not use damaged components.
Caution! ( )
Device surface is partially made of glass!
› Glass surface can be damaged by impact.
› If glass surface is damaged it could cause injury,
do not use the device anymore.

10 Safety instructions
/// Permissible medium /
contaminants / side reactions
Warning! ( )
Beware of hazards due to:
› flammable materials
› glass breakage
› incorrect container size
› overfilling of media
› unsafe condition of container
Danger! ( )
Only process media that will not react dangerously to the extra energy
produced through processing. This also applies to any extra energy produced
in other ways, e.g. through light irradiation.
› The stir plate can heat up due to the action of
the magnets at high motor speeds.
› Please consider any possible contaminations and unwanted
chemical reactions.
› It may be possible for wear debris from rotating accessory parts
to reach the material being processed.
/// Experimental procedures
Warning! ( )
Wear your personal protective equipment in accordance with
the hazard category of the media to be processed.
There may be a risk from
› splashing and evaporation of liquids
› ejection of parts
› release of toxic or combustible gases

Safety instructions 11
Reduce the stirring speed, if
› the medium splashes out of the vessel because the speed is too high.
› the device is not running smoothly.
›the container moves on the stirring plate.
›an error occurs.
/// Accessories
› Safe operation is only guaranteed with the accessories described in the
"Accessories" chapter.
› Always disconnect the plug before attaching or removing accessories.
› Observe the operating instructions of the accessories.
› Ensure that the external temperature sensor is inserted into the medium to
a depth of at least 20 mm when connected.
› Accessories must be securely attached to the device and must not come
off by themselves. The center of gravity of the assembly must lie within the
surface on which it is set up.
›External temperature probes can react with the medium and cause a
short-circuit.
1. It is important to use a sensor that is isolated against electricity. Our
recommendation is to use temperature probe PT 1000.90 (xxxx). Please
ensure that the coating is resistant to the solvent being used and in an
undamaged condition.
2. A non-insulated or not fully coated temperature sensor can seriously
damage or destroy ElectraSyn 2.0. Measuring outside of the vial, e.g. inside
a dry block, a metal probe can be used.

12 Proper usage
/// Power supply / Switching off
› The voltage stated on the type plate must correspond to the mains voltage.
› The socket for the power cord must be easily accessible.
› The device can only be disconnected from the power supply by pulling out
the power plug or the connector plug.
/// Protecting your device
› This device should only be disassembled by qualified IKA personnel.
› Protect the device and accessories from bumps and impacts.
› Keep base plate clean.
Proper usage
/// Basics
Usage
› The potentiostat IKA ElectraSyn 2.0 has been designed for electrochemical
reactions and mixing.
› Unpack the device carefully. Any damage to the exterior packaging
should immediately be reported to the carrier (mail, rail or freight
forwarding company).
Area of use (only indoors)
› The device is suitable for use in residential areas and all other areas.
The safety of the user cannot be ensured, if
› the device is used in conjunction with accessories not made or recommen-
ded by the manufacturer!
› modifications to the device or parts of the device are made by third parties!
› the device is operated in violation of the safety instructions!

Start-up 13
Start-up
/// Your ElectraSyn package
Unpack the device carefully. Any damage should immediately be
reported to the carrier (mail, rail or freight forwarding company).
PREPARE STATION
SCOPE OF DELIVERY
Place single vial adapter on plate.
Note: The front of the vial adapter needs to
be in line with the edge of the glass plate
Turn and engage (click)
Single vial holderElectraSyn 2.0 base unit Power plug
IKA stir plate
Set of electrodes and single vial
1

14 Start-up
Attach lid to vial
PREPARE VIAL
Put IKA FLON into vial
Insert electrodes into lid
Place vial on plate (connection)
PLUG
2
3

Start-up 15
Setting up a reaction
/// Basic guide
1. Turn on ElectraSyn 2.0
2. Select "new experiment"
3. Choose experiment type (constant voltage or constant current)
4. Indicate if a reference electrode will be used (note: if no reference electrode
will be used, the voltage displayed will be the potential difference between
the working and counter electrode)
5. Set the voltage/ current desired (note: if unsure of the voltage /current
assist mode can be used to approximate reaction conditions)
6. Set duration of experiment
›Total charge duration will run the reaction until the set charge has
passed, based on mmol of substrate and equivalents of electrons
(F/ mol)
›Timer will run the reaction for set amount of time
›Run continuous will run the reaction until the user manually stops
the reaction
7. Indicate if you would like to alternate the polarity of the electrodes during
the reaction (note: this feature is used for reactions where electrode fouling
can occur and can help certain reactions avoid some of these issues. This
feature should only be used when the anode & cathode are the same
electrode material)
8. Save the experiment parameters if desired.
9. The experiment parameters are now displayed in the edit screen. Select
"start" to begin experiment, or select "edit" to edit any of the parameters.

16 Start-up
Smart Assist
/// Take the guesswork out of Electrochemistry
The Smart Assist feature on the ElectraSyn 2.0 is designed to guide a new
user through the steps of setting up an electrochemical reaction. In addition,
more experienced users may find this feature useful to determine appropriate
current levels when running a reaction for the first time.
Smart Assist works by determining the current needed to achieve a cell
potential the corresponding power level selected by the user. Power level
"low", "medium" and "high" correspond to cell potentials of 2, 4 and 6 volts
respectively (without reference electrode). For example, selecting power level
"medium" will allow the ElectraSyn 2.0 to determine the current needed for
a starting potential of 4 V. The current determined will then be used to run a
constant current electrolysis reaction. The experiment duration for Smart As-
sist is determined by calculating the charge needed based on the user’s input
of # mmol of substrate, and the desired equivalents of electrons (F / mol).
When using Smart Assist, it is recommended to start with power level
"medium". If no reaction is observed, power level "high" can be used, while
if over-oxidation/reduction is observed, power level "low" should be used.
Further optimization of reaction conditions can be carried out by beginning
a new experiment or by editing the reaction parameters using the "edit"
function in Smart Assist.
4 mA!

Start-up 17
Cyclic Voltammetry
/// Scope of delivery
/// Reference Electrode (RE)
The reference electrode is delivered in “dry” form. One of the most common
types of electrolyte for this electrode is aqueous 3 M KCl. However, different
solutions of interest could be used as electrolyte as well. For example, a solu-
tion of perchloric acid (HClO4) should use 3 M NaCl as reference electrolyte,
since potassium perchlorate (KClO4) is a sparingly soluble salt and it may
deposit on the frit. For measuring non-aqueous solutions, aqueous 3 M KCl
is compatible in most cases. However it is not advisable to use the reference
electrode continuously for an extended period of time, as there might be
crystallization on KCl on the frit. If needed, non-aqueous electrolyte such as
acetonitrile solution of AgNO3could also be applied.
After the electrode has been filled, it should be left inside a solution cont-
aining the same electrolyte to allow the frit to soak. After using the electrode,
rinse thoroughly with water or acetone (depending on the electrolyte used)
and immerse it in the previously mentioned solution. Another alternative
would be to fit it inside the rubber cap with a small volume of the electrolyte
inside.
To use the electrode, rinse it and insert it in the center hole of the cap (as
depicted in the picture), then twist it clockwise until secured.
Over time, the electrolyte solution will lose ions. In this case, empty the soluti-
on and refill by following the steps above.
Ag wire
reference electrode
3 mm diameter glassy
carbon disc electrode
(working electrode)
Platinum
plate electrode

18 Start-up
/// Working Electrode (WE)
The working electrode contains a glassy carbon disc which is 3 mm in diame-
ter. This surface will accumulate debris from its use in different reactions. To
ensure ecacy, it is recommended to re-polish it with high grit sand paper
(above 1200 grit). This electrode should be placed in the WE section of the
cap (There is also an indication of W and C at the top of a cap).
/// Counter Electrode (CE)
The counter electrode consists of a platinum coated copper substrate. It is not
recommended to sand this electrode as exposing the substrate might hinder
its functionality. This electrode should be placed in the CE section of the cap.
WE = Working Electrode
CE = Counter Electrode
RE = Reference Electrode
WE RE CE

Start-up 19
/// CV setup
ASSEMBLE REFERENCE ELECTRODE AND CV CELL
1
1. Remove Ag wire and electrode head from glass tube.
2. Fill tube to halfway point with electrolyte solution*
3. Insert Ag wire and electrode head into glass tube, the rubber seal should fit
snugly
4. Place assembled reference electrode in a tube containing the electrolyte solution
and let stand until glass frit is saturated
5. Attach reference electrode into ElectraSyn vial lid
6. Attach working electrode and counter electrode to ElectraSyn vial lid
(note, "W" and "C" on top of vial lid correspond to position working
electrode and counter electrode orientation)
7. Attach lid onto vial
8. Add CV sample to vial via top cap (note: solution level should be high enough in
the vial to submerge the working electrode and reference electrode tips by ~5 mm)
*A standard electrolyte solution is 3 M KCl(aq.); however, other electrolytes and elect-
rolytes in organic solutions can also be used in the ElectraSyn reference electrode.

20 Start-up
RUNNING A CV EXPERIMENT
2
Example of CV parameters
Segment: 3 | Initial V: 0.0 | Direction: Rising | Upper V: 1.5 | Lower V: -1.0 | Final V: -0.1 | Sweep (mV/sec): 400
Current (A)
Potential (V)
lower final initial
segment 3 segment 1
segment 2
upper
1. Turn on ElectraSyn 2.0
2. Select "new experiment"
3. Select "Cyclic Volatametry" (Note: the CV experiment can alternatively be acces-
sed by pressing the "CV" button
4. Select "start" to begin CV experiment using default settings. The CV graph screen
will be displayed and a blue line will move across the top of the screen indicating
the ElectraSyn 2.0 is collenting data. When finished the CV curve will be displayed
5. When CV is complete the data can be saved to USB drive
6. To edit CV parameters, select "edit"
7. CV parameters can be modified by selecting "edit" and editing as desired
(starting, upper, lower and end voltage, sweep rate etc.)
Tips
› Surface of working electrode is clean and flat.
› Working and counter electrodes are placed correctly.
› Enough amount of electrolyte (0.05 M – 0.5 M) is included in a sample solution.
› Concentration of a sample is appropriate (1 mM – 10 mM)
› Solvent is unreactive within scan range.

Technical data 21
Technical data
/// ElectraSyn 2.0 in detail
Technical data ElectraSyn 2.0
Potentiostat
Nominal voltage 48 VDC
Max. power input 36 W
Power input standby 5 W
Voltage output (electrode) 30 / 10 V
Current output (electrode) 100 mA
Motor rating output 9 W
Speed range 50 - 1500 rpm
Setting accuracy speed 10 rpm
Stirring quantity max. per stirring position (H2O): 100 ml
Length of stirring bar 20 mm
Display TFT
USB port yes
RS-232 interface no
Analogue output no
Protection class to DIN EN 60529 IP 40
Permissible ambient temperature + 5 … + 40 °C
Permissible relative humidity 80%
Dimensions incl. glass vessel adapter (W x H x D) 130 x 150 x 250 mm
Weight 1.5 kg
AC adapter x D)
Input
100 – 240 VAC
0.75 A
50 – 60 Hz
5 W
48 VDC
Output 48
39.84 W LPS (Limited Power Source)
Protection class II (double insulated)