910 PSTAT mini

PSTAT Software

Manual
0 Conformity and warranty

0.1 Declaration of Conformity

This is to certify the conformity to the standard
specifications for electrical appliances and accessories, as
well as to the standard specifications for security and to
system validation issued by the manufacturing company.
______________________________________________

Name of commodity 910 PSTAT mini

Instrument for electrochemical research and voltammetric
analyses.
______________________________________________

This instrument has been built and has undergone final

type testing according to the standards:

Electromagnetic Emission: EN/IEC 61326-1: 2006, EN/IEC 61000-6-3:2007,

Compatibility CISPR 11: 2008
Immunity: EN/IEC 61326-1: 2006, EN/IEC 61000-6-1: 2007,
EN/IEC 61000-4-2: 2001,
EN/IEC 61000-4-3: 2006

This instrument meets the requirements of the CE mark as

contained in the EU directives 2006/95/EC (LVD),
2004/108/EC (EMC). It fulfils the following specifications:

EN 61326-1 Electrical equipment for measurement,

control and laboratory use – EMC
requirements

Manufacturer Metrohm Ltd., CH-9101 Herisau/Switzerland

 Metrohm Ltd. is holder of the SQS certificate ISO
9001:2008 Quality management system for development,
production and sales of instruments and accessories for
ion analysis.

Herisau, 07 September, 2010

D. Strohm A. Dellenbach
Vice President, Head of R&D Head of Quality Management

0.2 Warranty (guarantee)

Metrohm guarantees that the deliveries and services it
provides are free from material, design or manufacturing
errors. The warranty period is 36 months from the day of
delivery; for day and night operation it is 18 months. The
warranty remains valid on condition that the service is
provided by an authorized Metrohm service organization.
Glass breakage is excluded from the warranty for
electrodes and other glassware. The warranty for the
accuracy corresponds to the technical specifications given
in this manual. For components from third parties that
make up a considerable part of our instrument, the
manufacturer's warranty provisions apply. Warranty
claims cannot be pursued if the Customer has not
complied with the obligations to make payment on time.
During the warranty period Metrohm undertakes, at its
own choice, to either repair at its own premises, free of
charge, any instruments that can be shown to be faulty or
to replace them. Transport costs are to the Customer's
account.
Faults arising from circumstances that are not the
responsibility of Metrohm, such as improper storage or
improper use, etc. are expressly excluded from the
warranty.
0.3 Quality Management Principles
Metrohm Ltd. holds the ISO 9001:2008 Certificate,
registration number 10872, issued by SQS (Swiss
Association for Quality and Management Systems).
Internal and external audits are carried out periodically to
assure that the standards defined by Metrohm’s QM
Manual are maintained.
The steps involved in the design, manufacture and
servicing of instruments are fully documented and the
resulting reports are archived for ten years. The
development of software for PCs and instruments is also
duly documented and the documents and source codes
are archived. Both remain the possession of Metrohm. A
non-disclosure agreement may be asked to be provided by
those requiring access to them.
The implementation of the ISO 9001:2008 quality
management system is described in Metrohm’s QM
Manual, which comprises detailed instructions on the
following fields of activity:
Instrument development
The organization of the instrument design, its planning
and the intermediate controls are fully documented and
traceable. Laboratory testing accompanies all phases of
instrument development.
Software development
Software development occurs in terms of the software life
cycle. Tests are performed to detect programming errors
and to assess the program’s functionality in a laboratory
environment.
Components
All components used in the Metrohm instruments have to
satisfy the quality standards that are defined and
implemented for our products. Suppliers of components
are audited by Metrohm as the need arises.
Manufacture
The measures put into practice in the production of our
instruments guarantee a constant quality standard.
Production planning and manufacturing procedures,
maintenance of production means and testing of
components, intermediate and finished products are
prescribed.
Customer support and service
Customer support involves all phases of instrument
acquisition and use by the customer, i.e. consulting to
define the adequate equipment for the analytical problem
at hand, delivery of the equipment, user manuals,
training, after-sales service and processing of customer
complaints. The Metrohm service organization is equipped
to support customers in implementing standards such as
GLP, GMP, ISO 9001, in performing Operational
Qualification and Performance Verification of the system
components or in carrying out the System Validation for
the quantitative determination of a substance in a given
matrix.
 910 PSTAT mini Manual

Contents

1. Introduction .................................................................. 1
2. Recommendations ......................................................... 2
2.1. Voltage overload and Current underload or overload........2
2.2. Resolution and optimal current range selection ...............2
2.3. Noise ........................................................................2
3. Getting started: Installation and Setup.......................... 4
3.1. Installation of the software ..........................................5
3.2. Connecting to 910 PSTAT mini......................................5
3.3. Test with dummy cell ..................................................5
4. Measuring ...................................................................... 6
4.1. Readings ...................................................................6
4.2. Parameters................................................................6
4.3. Limits of some technique specific parameters .................9
4.4. Validation ..................................................................9
4.5. Running a measurement............................................ 10
5. Curves ......................................................................... 11
5.1. Plot ........................................................................ 11
5.2. Measurements ......................................................... 14
5.3. Curve files ............................................................... 15
6. External Digital and Analog I/O................................... 16

7. 910 PSTAT mini instrumental specifications ................ 18

7.1. Firmware update ...................................................... 18
1. Introduction

910 PSTAT mini is a hand-held USB powered instrument for use with
electrochemical sensors or electrochemical cells. The instrument contains a
microprocessor which controls the potential applied to the sensor and
measures the current response.
In general, the instrument is used with electrochemical sensors or
electrochemical cells with three electrodes: working electrode, reference
electrode and auxiliary electrode. Also, it can be used in bipotentiostat
mode, with a two-working electrodes system, a reference electrode and an
auxiliary electrode. 910 PSTAT mini can be connected to a PC by means of a
USB cable.

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2. Recommendations

2.1. Voltage overload and Current underload or overload

User must take precautions with current overload, current underload or
voltage overload.
Voltage overload can be found when:
- the auxiliary or the reference electrode is not properly connected,
- the conductivity of the solution is too low, which is overcome by adding an
electrolyte,
- an air bubble isolates the reference electrode from the solution.
Measured current values are wrong when a current overload is detected.
This occurs when the current is below -2 or above +2 times the applied
current range.
If currents are below 0.05 of the selected current range, a current
underload occurs, since a lower current range can be applied. An underload
will yield measurements with a low resolution.

2.2. Resolution and optimal current range selection

The resolution of the measurements of the potential is 1 mV and of the
current equal to 0.01 times the applied current range. The measurement
range is -2.000 V to +2.000 V and -2 to +2 times the applied current
range. The best way of obtaining an optimal current measurement
resolution is to use autoranging (Current Range: Auto). A higher current
range is selected when the current exceeds 2 times the applied current
range. A lower current is selected when the measured current is lower than
0.05 times the applied current range. The selectable current ranges are
specified in the ‘Method’ tab.

2.3. Noise
Electrochemical sensors and cells are susceptible to noise.
Known sources of noise are:
- AC-adapters. Laptop adapter induces noise. Sensitive measurements must
be performed without these adapters connected.

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- Electrical equipment. Measurements in the vicinity of electrical equipment
might be distorted by electrical interference. This might be eliminated by
placing the cell in a faraday cage which is connected to earth or ground.
- Unshielded or too long electrode- or cell cables. The connection between
910 PSTAT mini and the sensor or cell should not be extended. Especially
unshielded cables used with many commercially available reference
electrodes may result in high noise levels. Shorten the cables when
possible.
In case the noise levels remain too high, the use of a faraday cage is
required. Connect the metal cage to safety ground or to the green
connector of the 910 PSTAT mini electrode cable.

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3. Getting started: Installation and Setup

Requirements:
- Windows PC or laptop, preferably with Windows XP, Vista or 7.
- Screen resolution of 1024 x 768 minimum and 1280 x 1024 advised
- USB cable (included) [6.2151.110]
- 910 PSTAT Software installation CD-ROM (included)
- 910 PSTAT mini instrument (included)
- Electrode cable (included) [6.2163.000]
- Dummy cell (included) [3.910.3020]
- Dummy cell cable (included) [6.2163.010]
- Crocodile clamps (5 x included)

Instrument:

ELECTRODE STATUS I/O USB

Front view Rear view

ELECTRODE: Connector for electrode cable

STATUS: LED indicator
I/O: Connector for remote cable (not included) [6.2163.020]
USB: Connector for USB cable

Electrode cable colour codes:

R
Reed
d - working electrode 1 (WE1)
Y
Yeellllo
oww - working electrode 2 (WE2)
Black - auxiliary electrode (AE)
B
Bllu
uee - reference electrode (RE)
G
Grreeeen
n - ground ( )

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LED indicator colour:
Green – 910 PSTAT mini is switched on
Orange – Measuring
Red – Overload detected

3.1. Installation of the software

1.- Insert the CD ROM. A Menu is automatically displayed.
2.- Select the options of your choice. Install the program by clicking on
“Install PSAT Software”. After installation, a 910 PSTAT Software
shortcut is placed on the desktop.
The USB driver is automatically installed after software installation. This
may take some seconds; during installation, a black window is displayed.

3.2. Connecting to 910 PSTAT mini

Plug in the 910 PSTAT mini to the USB port.
Run 910 PSTAT Software.
Press the “Connect to device” button
910 PSTAT mini is connected when the “Disconnect from device” button is
available and led light in 910 PSTAT mini is green.
Establish connection to 910 PSTAT mini each time you run 910 PSTAT
Software.

3.3. Test with dummy cell

Perform an initial test of the instrument with the dummy cell. Follow the
next steps:
1.- Connect the dummy cell to the potentiostat using the dummy cell cable.
2.- Open the “dummy_test” method in the route C:\Program
Files\Metrohm\PSTAT Software\Examples.
3.- Run the measurement (see 4.1) and check that the recorded curve is
similar to the one displayed by the “dummy_test” file.

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4. Measuring

4.1. Readings
The instrument is controlled manually using the ‘Method’ tab (see 4.2).
Click the “New” method button in the toolbar to select the technique
to be used.
Tick the “Bipotentiostat” option if you want to work in bipotentiostat mode.
Tick the “Leave cell on” option if you want to leave cell on after
measurement.
Select the parameters of the technique and the current range (see 4.2).
Click “Run” button to start the measurement. Led light in 910 PSTAT
mini turns orange during measurement.

4.2. Parameters
910 PSTAT Software provides the possibility to apply some relevant
voltammetric techniques. The program also provides the possibility to
measure current as a function of time. The applicable techniques are:

Voltammetric techniques:
■ Linear Sweep Voltammetry LSV
■ Cyclic voltammetry CV
■ Square Wave Voltammetry SWV
■ Differential Pulse Voltammetry DPV

Amperometric techniques:
■ Amperometric Detection AD
■ Pulsed Amperometric Detection PAD

The ‘Method’ tab contains all the technique parameters.

The ‘Sensor’ and ‘Sample’ textboxes can be used to describe the sensor
used and the sample that is measured.

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 Figure 1 - Method parameters tab

With the “Current range” frame, the applicable current range during the
measurement can be selected. If “Auto” is selected, the instrument will
select the most optimal current range automatically.

Parameters of voltammetric techniques:

Pretreatment
Econd Potential applied before the deposition stage is started. It is
only relevant when tcond > 0 s.
Edep Potential applied during the deposition stage. It is only relevant
when tdep > 0 s.
tcond Conditioning time.
tdep Deposition time.
tequil Equilibration time. During this stage Ebegin is applied.

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Measurement
Ebegin Potential where scan starts. The applicable range of the
potential is -2 V to +2 V.
Evtx1 (CV) Potential where scan direction is reversed. The applicable
range of the potential is -2 V to +2 V.
Evtx2 (CV) Potential where scan direction is reversed again or where
scan stops (if Evtx2 = Ebegin). The applicable range of the
potential is -2 V to +2 V.
Eend Potential where scan stops.
Estep Step potential.
Eamp (SWV) Amplitude of square wave pulse.
Epuls (DPV) Pulse potential.

Srate Applied scan rate.

nscans (CV) Number of scans.
Freq (SWV) Frequency.
tpuls (DPV) Pulse time.

The sequence of a measurement is:

- Apply Econd, the conditioning potential, if tcond is not zero.
- Apply Edep, the deposition potential, if tdep is not zero.
- Apply Ebegin and wait tequil seconds.
- Start measurement at Ebegin and continue until Eend with steps Estep,
with the specified Scan rate. In CV the scan starts at Ebegin and is
continued by reversing the scan direction at Evtx1. Scan direction is
reversed again if Evtx2 is different from Ebegin.

Parameters of amperometric techniques:

Pretreatment
Econd Potential applied before the deposition stage is started. It is
only relevant when tcond > 0 s.
Edep Potential applied during the deposition stage. It is only relevant
when tdep > 0 s.
tcond Conditioning time.
tdep Deposition time.
tequil Equilibration time. During this stage Ebegin is applied.

Measurement
E (AD) Potential during measurement. The applicable range of
the potential is -2 V to +2 V.
Interval (AD) Time between two measurements.
E1,2,…,5 (PAD) Potential pulses (applied during their corresponding
t1,2,…,5).
Ei (PAD) Integration potential (applied during ti).
t1,2,…,5 (PAD) Potential pulse times (at their corresponding E1,2,…5).

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ti (PAD) Integration time (at Ei).
t Total time of measurement.

The sequence of a measurement in AD is:

- Apply Econd, the conditioning potential, if tcond is not zero.
- Apply Edep, the deposition potential, if tdep is not zero.
- Apply E and wait teq seconds.
- Start the measurement at E during t seconds.

The sequence of measurement in PAD is:

- Apply Econd, the conditioning potential, if tcond is not zero.
- Apply Edep, the deposition potential, if tdep is not zero.
- Apply E1 and wait teq seconds.
- Start the measurement following the potential waveform in the order
1,2,3,4,5,i as follows:
Apply Potential pulses E1,2,…5 during their corresponding times t1,2,…5
(if a t is zero, its potential pulse is not applied); current is registered at Ei
during ti.

4.3. Limits of some technique specific parameters

LSV and CV Scan rate: 1 mV/s to 5.0 V/s

Frequency: 1 Hz to 400 Hz
SWV
Amplitude: 1 mV to 250 mV
Scan rate: 1 mV/s to 2.5 V/s
DPV
Pulse time: 1 ms to 200 ms
Interval time: 100 ms to 1300 s
AD
Run time: Hours (65000 points)
Pulse time: 1 ms
PAD
Run time: Hours (65000 points)

4.4. Validation
After every changed parameter the method is automatically validated for
errors. These errors are shown in red in the parameter textbox and
explained in the textbox below the ‘Method’ tab.

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4.5. Running a measurement
Measurements can be started, paused and stopped with the buttons in the
toolbar .

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5. Curves

5.1. Plot
Curves are shown in the Plot window.

Figure 2 - Plot window

The “Curves” tab displays the curve list of curves shown in plot.
Curve width can be changed with the “Line width” option in View menu.
Curves can be visible or not by clicking on the eye icon next to the curve
name.
Curve name can be changed by slow double clicking on the curve name.
Curve colour can be changed clicking on the coloured square next to curve
name.
If “Erase previous curves” is selected, displayed curves are deleted when a
new scan starts. If it is not selected, curves recorded in a new scan overlay
the displayed curves.

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 Figure 3 - Curves tab

Curves can be deleted with “Erase non visible” and “Erase all” buttons.
After selecting one curve, “Substract curve…” allows you to substract other
of your choice among those displayed in Curves list.
“Smooth” allows you to apply Savitzky-Golay smoothing to the selected
curve.
Data of selected curve can be exported to a *.csv file with “Export
selected…” button or can be copied to clipboard with “Copy to clipboard”
button.
Plot window can be printed or saved as a *.png image file with the “Print…”
and “Export image…” options, respectively, in File menu.

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The toolbar allows the user to work with the curves:

Plot

Manually Edit Axis scales

Enter minimum and maximum values for both axes.

Autoscale axis
Scales automatically the plot window to fit the displayed curve.

Show grid
Shows grid in plot window.

Show legend
Shows legend in plot window.

Zoom tool
Zooms the selected area of plot window.

Peaks or levels

Peak measurement tool 1

Mark peaks (curve baseline). Click to select; right click to
unselect.

Peak measurement tool 2

Mark peaks (free baseline). Click to select; right click to unselect.

Step measurement tool

Mark levels. Click to select; right click to unselect. To measure a
level, first mark the baseline (2 points) and then select the
highest point of the level.

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 Automatic peak measurement tool
Mark peaks (automatic). Click to mark all the relevant peaks
automatically.

Clear all measurements

Removes peak marks.

Export as PNG
Exports the plot window to a *.png image file.

5.2. Measurements
Peak data are shown in “Measurements” tab. Each peak is labelled and data
are displayed below its corresponding curve name.

Figure 5 - Measurements tab

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“Export” button allows you to export the measurement results to a *.csv
file.

5.3. Curve files

Curves and/or method parameters files are saved with different extensions
for each technique. The extensions are as follows:
*.mtl: Linear Sweep Voltammetry.
*.mtc: Cyclic Voltammetry.
*.mts: Square Wave Voltammetry.
*.mtd: Differential Pulse Voltammetry
*.mta: Amperometric Detection.
*.mtp: Pulsed Amperometric Detection.

It is possible to:
- save registered curves and the method parameters associated to that
curves (“Save” and “Save as…” options in File menu),
- save only the curves (visible) but not the method parameters associated
to that curve (“Save visible curves…” option in File menu),
- save only the method parameters displayed in the “Method” tab (“Save
parameters…” option in File menu).
It is also possible to:
- open all the data recorded in one file, i.e. curves and/or method
parameters (“Open…” option in File menu or in the toolbar ),
- open only the method parameters recorded in one file (“Load
parameters…” option in File menu),
- open only the curves recorded in one file (“Load curves…” option in File
menu or in the toolbar ).
To open and overlay curves from different files, open the curves with the
“Load curves…” option in File menu or in the toolbar.

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6. External digital and analog I/O
The Digital and Analog Inputs/Outputs can be configured with the
“Peripheral Configuration” option in Device menu. The displayed window
allows you to enable or not the desired Programmable I/O (PIO) pins.

Figure 6 – Setup IO pins window

The “IO Type” option allows you to select a Digital input, Digital output or
Analog input.
If Digital output or Digital input is enabled, you can select “Active Level”
High (signal) or Low (no signal) and associate an “Event” when this level
occurs. The available events are:

OUTPUT INPUT
Run Run
Stop Stop
Pause Pause
Conditioning time Skip to next phase
Deposition time
Equilibration time
Measurement

16
If “Analog Input” is enabled, the input voltage versus time is registered and
displayed in an emerging window. Registry starts with the beginning of the
potentiostat measurement. The allowed voltage range for the “Analog input”
is from 0 to 5 V, with 5 mV precision.

If “Analog Output” is enabled, the current registered in WE1 is sent in

voltage (from 0.048 V to 4.048 V) through the pin.
Current range must not be set in “Auto” if “Analog Output” is used, but in
any of the six fixed current ranges.
The voltage sent for 0 A is always 2.048 V and the voltage/current scale is
always 1V/(current range). The following examples show the voltage sent
depending on the selected current range:

Current range Current range

10 μA 100 nA
Registered Sent Registered Sent
Current Voltage Current Voltage
+ 20 μA 0.048 V + 200 nA 0.048 V
+ 10 μA 1.048 V + 100 nA 1.048 V
0 μA 2.048 V 0 nA 2.048 V
- 10 μA 3.048 V - 100 nA 3.048 V
- 20 μA 4.048 V - 200 nA 4.048 V

The pins position in the I/O connector is shown in the next Figure:

8 7 6 1: Ground 5: PIO 5
2: I-Out 6: PIO 1
5 4 3
3: +5 V 7: PIO 2
2 1 4: PIO 4 8: PIO 3

Figure 7 – I/O Connector

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7. 910 PSTAT mini instrumental specifications

- Power 5 V / 45 mA max. USB powered

- PC interface USB
- DC-potential range ± 2.048 V
- Current ranges 1 nA to 100 µA (6 ranges)
- Maximum measurable current 200 µA
- Rise time 20 µs
- Current resolution 0.5 % of current range
10 pA on lowest current range
- DC-potential resolution 1 mV
- DC-offset error ± 1 mV
- Accuracy ≤ 0.1 %
- Electrometer amplifier input CMOS input, C<2 pF
- Extra inputs/outputs • 5 generic digital I/O pins (5 V TTL)
[PIO 1, PIO 2, PIO 3, PIO 4 , PIO 5:
Digital input/Digital output]
3 10-bit ADC inputs multiplexing PIO
1, PIO 2, PIO 3
[PIO 1, PIO 2, PIO 3: Analog input (0
to 5 V, precision 5 mV)]
• I-out: Analog output for cell current
monitoring. From 0.048 V to +4.048
V
• 0 V and +5 V supply outputs
- Dimensions 8.0 cm x 5.4 cm x 2.3 cm (L x W x H)

7.1. Firmware update

Firmware can be updated with available updates (*.hex file). To update
firmware, plug in the 910 PSTAT mini to the USB port; select “Update
firmware…” in the Device menu and browse for the corresponding *.hex
file; click “Upload” button and wait until update is finished successfully. Do
not unplug the 910 PSTAT mini while update is in progress.

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