IKA ElektraSyn 2.0 User Manual

ElektraSyn 2.0

Declaration of conformity

We declare under our sole responsibility that this product corresponds to the regula­tions 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
[e-mail].

/// 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

4

/// SETTING UP A REACTION

Basic guide . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16

›

/// SMART ASSIST

Take the guesswork out of Electrochemistry . . . . . . . . . . . 16

›

/// CYCLIC VOLTAMMETRY

Scope of delivery. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17

›
›

Reference Electrode (RE) . . . . . . . . . . . . . . . . . . . . . . . . . 17

Working Electrode (WE). . . . . . . . . . . . . . . . . . . . . . . . . . 18

›
›

Counter Electrode (CE). . . . . . . . . . . . . . . . . . . . . . . . . . . 18

› CV setup. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19

/// TECHNICAL DATA

›

ElectraSyn 2.0 in detail . . . . . . . . . . . . . . . . . . . . . . . . . . 21

/// WARRANTY

› Regulations. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22

5

Device setup

/// ElectraSyn 2.0

LM

Explication of symbols

A ON / OFF switch (standby)

B Rotating knob (chose values / start-stop)

C "Menu" button

D "Cyclic Voltammetry" button

E "Back" button

F "Graph" button

G "Lock" button

6 Device setup

H

BCFGEDA

H Display

I Power socket

J Contact thermometer jack

K Micro USB interface

L Threaded hole for vertical rod

M Single vial holder

JKI

/// Display

07 08 09 10 11 12 1413

15

Display

02

03

0105 0406

01 Set speed

02

03

04 Charge activated

05 Motor activated

06 Timer / remaining charge

07 Polarity indicator

08

Actual / set voltage
(depending on selected operating mode)

Actual / set current
(depending on selected operating mode)

Actual temperature
(in connection with an external PT1000 sensor)

Operation mode

09

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

(constant voltage / constant current)

Estimated duration of experiment /
charge counter

Device setup 7

Safety instructions

/// Explication of warning symbols

Indicates an (extremely) hazardous situation, which,
if not avoided, will result in death, serious injury.

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.

!

Indicates practices which, if not avoided, can result in
equipment damage.

Attention!

- risk of damage due to magnetism.

DANGER!

- note on hazards arising from a hot surface.

8 Safety instructions

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.

)

Safety instructions 9

/// 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

10 Safety instructions

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

ccessories" chapter.

"A

› Always disconnect the plug before attaching or removing accessories.
› Observe the operating instructions of the accessories.
› Ensure that the external temperatur

a depth of at least 20 mm when connected.

› Accessories must be secur

off by themselves. The center of gr

surface on which it is set up.

External temperature probes can react with the medium and cause a

›

short-circuit.

ely attached to the device and must not come

e sensor is inserted into the medium to

avity of the assembly must lie within the

1. It is important to use a sensor that is isolated against electricity. Our

r

ecommendation is to use temperature pr
ensure that the coating is resistant to the solvent being used and in an
undamaged condition.

2. A non-insulated or not fully coated temperatur
damage or destr
a dry block, a metal probe can be used.

oy ElectraS

yn 2.0. Measuring outside of the vial, e.g. inside

obe PT 1000.90 (xxxx). Please

e sensor can seriously

Safety instructions 11

/// 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!

12 Proper usage

Start-up

/// Your ElectraSyn package

Unpack the device carefully. Any damage should immediately be

reported to the carrier (mail, rail or freight forwarding company).

SCOPE OF DELIVERY

IKA stir plate

1

PREPARE STATION

Single vial holderElectraSyn 2.0 base unit Power plug

Set of electrodes and single vial

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

Start-up 13

Turn and engage (click)

2

PREPARE VIAL

Insert electrodes into lid

Put IKA FLON into vial

3

PLUG

Attach lid to vial

Place vial on plate (connection)

14 Start-up

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.

Start-up 15

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 As­sist 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.

16 Start-up

4 mA!

Cyclic Voltammetry

/// Scope of delivery

Ag wire

reference electrode

3 mm diameter glassy

carbon disc electrode

(working electrode)

Platinum

plate electrode

/// 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 solu­tion 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 AgNO

could also be applied.

3

After the electrode has been filled, it should be left inside a solution cont­aining 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 soluti­on and refill by following the steps above.

Start-up 17

/// Working Electrode (WE)

The working electrode contains a glassy carbon disc which is 3 mm in diame­ter. 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

RE CE

WE = Working Electrode
CE = Counter Electrode
RE = Reference Electrode

18 Start-up

/// 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

; however, other electrolytes and elect-

(aq.)

rolytes in organic solutions can also be used in the ElectraSyn reference electrode.

Start-up 19

2

RUNNING A CV EXPERIMENT

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.)

segment 3 segment 1

Current (A)

segment 2

lower final initial

Potential (V)

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

upper

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.

20 Start-up

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)

100 – 240 VAC

0.75 A

Input

50 – 60 Hz
5 W
48 VDC

Output

Protection class II (double insulated)

48

39.84 W LPS (Limited Power Source)

Technical data 21

Warranty

/// Regulations

According to IKA’s terms and conditions this product carries a lifetime
warranty. For warranty claims, please contact your local IKA oce. You can
also send your device directly to IKA, including the invoice and explaining your
claim. Please note that you will be responsible for the shipping costs.

The warranty does not cover worn out parts, nor does it apply to problems
resulting from improper use, insucient care or maintenance not carried
out in accordance with the instructions in this operating manual.

22 Warranty