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Connection of SEC2020 and Potentiostat

Here, the SEC2020 Spectrometer connection with some potentiostat using trigger cable, which is one of the content of the system package, is introduced below.

Trigger mode measurement

The spectrometer supports Trigger Mode for synchronized measurement with external device. Depending on the trigger mode, you can control acquisition of spectrometer data with external Input/Output signal. It makes possible to control the spectrometer measurement with external operation of the external devices.

  • Configuration
  • Cable connection
  • SEC-C setting
  • Synchronized measurement

Configuration

The electrochemical measurement synchronized with a spectrum monitoring is introduced in this section.

SEC2020 Spectrometer system

The electrochemical reaction is performed using Interface 1010ETM from Gamry Instruments, and the spectrum monitoring is performed using SEC2020 Spectrometer system.
The instruments and the respective accessories, and the reaction chamber, in this case the SEC-C Thin Layer Quartz Glass Spectroelectrochemical cell kit are listed below.

SEC2020 Spectrometer system

Catalog No. Description Spectrometer system content;(1) Spectrometer;(1a) Protector of the SMA 905 from the spectrometer;(2) Light source;(2a) Protector of the SMA 905 from the light source;(3) Cuvette holder;(4) Fiber collimator; (5) SMA905 adaptor for light shielding;(6) SEC2024 Platform;(7) Trigger cable
013609 SEC2020 Spectrometer system
Contents
(1) SEC2021 Spectrometer
(2) SEC2022 Deuterium halogen light source
(3) SEC2023 Cuvetter holder
(4) Fiber collimator
(5) SMA905 adaptor for light shielding
(6) SEC2024 Platform
(7) Trigger cable


Interface 1010ETM

Catalog No. Description Connection using single cables for the explanation of the connection. (1) Red cable (Analog Output High (The auxiliary output signal (DAC output))) and (2) Black cable (Analog Output Low (The auxiliary output ground connection (ground))
- Interface 1010E Potentiostat/Galvanostat/ZRA
- Multipurpose User I/O Cable
For information about the
Interface 1010ETM Potentiostat/Galvanostat/ZRA
contact Gamry Instruments

Interface 1010ETM from Gamry Instruments is used for the electrochemical measurement, for detailed information about the products, contact Gamry Instruments directly.
For the trigger connection the Multipurpose User I/O Cable is recommended.
This time, for the explanation set up, two pieces of single wire are used for the best visualization of the connection to the out put terminal.


SEC-C Thin Layer Quartz Glass Spectroelectrochemical cell kit

Catalog No. Description SEC-C Thin Layer Quartz Glass Spectroelectrochemical cell kit
013510 SEC-C Thin Layer Quartz Glass Spectroelectrochemical cell kit (Pt)
Contents
(011498) SEC-C Pt Gauze working electrode
(013703) SEC-C/C05 Pt counter electrode
(013512) SEC-C Thin Layer Quartz Glass cell
(011501) SEC-C Teflon cap
013613 RE-1BP Reference electrode (Ag/AgCl)
011840 IC clip for printed electrodes (4pcs)

The SEC-C Pt Gauze working electrode (Cat. No. 011498) connector wire is a 0.5 mm of the diameter platinum wire, which makes it very delicate and fragile. For the set up IC clip (Cat. No. 011840) is used to do not connect the crocodile clip directly to the connection wire of the SEC-C Pt Gauze working electrode.

Cable connection

Trigger cable (SEC2020 Spectrometer system content) and Multipurpose User I/O Cable (985-00171, from Gamry Instruments) are required for the connection.
For the explanation, instead of Multipurpose User I/O Cable, two single wires are used.

Connection of SEC2020 and Interface 1010E

SEC2020 Spectrometer system and Interface 1010E Potentiostat/Galvanostat/ZRA setting separately in the previous section is connected as shown below.

Connection of RRDE-3A and Model 2325 Fig. 7 Connection of the SEC2020 Spectrometer system and Interface 1010E Potentiostat/Galvanostat/ZRA


SEC2020 Spectrometer system Interface 1010E Potentiostat/Galvanostat/ZRA
① Brown (Input (Trigger-IN)

① Red cable (Analog Output High (The auxiliary output signal (DAC output))
② Black (Ground (GND))

② Black cable (Analog Output Low (The auxiliary output ground connection (ground))

SEC-C setting and connection

SEC-C Thin Layer Quartz Glass Spectroelectrochemical cell kit (Pt) (Cat. No. 013510) is used for the spectroelectrochemical measurement.
For the set up special care for the connection of the working electrode is necessary. In the below connection IC clip for printed electrodes (Cat. No. 011840) is connected to the crocodile clip.

Cell preparation for Spectrometry

Set up of the spectrometer and cuvette is showed below with some "hints".
For the SEC-C Thin Layer Quartz Glass Spectroelectrochemical cell kit (Cat. No. 013510) setting, first set the working electrode and counter electrode into the SEC-C Teflon cap, and then fit to the SEC-C Thin Layer Quartz Glass cell with the sample to be measured, and last set the reference electrode.
Make sure that the SEC-C Pt Gauze working electrode (Cat. No. 011498) is clean. If not, polish with 0.05 um polishing alumina (Cat. No. 012620) by soft touch using cotton swab, and rinse with distilled water.
For the spectrum measurement, when taking the reference and dark spectrum, do not forget to save both spectrum. The saved spectrum can be used for the subsequent measurement.
After take and save the reference and dark spectrum, SEC2020 Spectrometer system is ready for the target sample measurement.

Fig. 8 Reference spectrum for absorbance measurement.Fig. 8 For absorbance measurement, reference spectrum using distilled water. For a differential absorption spectrum, the spectrum of the sample before measurement is taking as a reference spectrum.
Fig. 9 Sample setting for absorbance measurement.Fig. 9 For absorbance measurement, as a measurement sample, 2 mM potassium ferricyanide/1 M KNO3 aqueous solution is used.


Setting of the cell cable

It is not recommended to clip the SEC-C Pt Gauze working electrode directly, because the connection wire is very thin and it will bend easily.
For the set up below IC clip for printed electrodes (Cat. No. 011840) is used between working electrode and cell cable.
For the connection of the working electrode, take attention to do not clip in the insulated side.

Fig. 9 Working electrode connection using IC clip.Fig. 9 Interface 1010E Potentiostat/Galvanostat/ZRA cell cable connection using IC clip. The connection must be in the exposed wire of SEC-C Pt Gauze working electrode, without the insulation.
Fig. 10 Cell cable connection.Fig. 10 IC clip is used between the crocodile clip of the Interface 1010E Potentiostat/Galvanostat/ZRA cell cable and exposed wire from the SEC-C Pt Gauze working electrode.

Set up of the devices - SEC020 Spectrometer system and Interface 1010

After finished the set up of the devices and the sample for the measurement is setting in the cuvette holder, the set up for the trigger measurement can be started.
For the spectrometry measurement the absorbance time sequence acquisition will be performed together with the cyclic voltammetry.

Spectra Smart (SEC2020 Spectrometer system)

Light source trigger

SpectraSmart can control the on/off states of an external light source via I/O signals.
Light source frame can be displayed on the right edge, where makes possible to control the type of the light, light on/off and shutter open/close.

Fig. 12 Starting the set up for light source control by the software.
Fig. 12 For the set up of the light source control by the software, first select the menu bar View and choose Light source to show the light source frame on the right edge of the window.
Fig. 13 Light source frame on the right edge of the window.
Fig. 13 Pressing the lamp at the light source frame, the operation mode is activated or inactivated.
Fig. 14 After activated the light source operation and the lights are turned on.
Fig. 14 After activated the light source operation, the lights are turned on. Also you can control the shutter to take the dark spectrum.

Reference and Dark spectrum

For the reference and dark spectrum, the data is taking for the set up Fig. 8 with distilled water.
Below, the reference and dark spectrum taking and saving step are explained in detail.
1. Setting Reference and Dark Spectrum
Before setting the test sample, take the reference and dark spectrum.

Fig. 15 Acquiring the reference spectrum.
Fig. 15 Acquire the reference spectrum, which can be acquired the live spectrum, or can be read the previously acquired and saved, using the Browse button.
Fig. 16 Acquiring the dark spectrum.
Fig. 16 Acquire the dark spectrum, closing the shutter (check the box, which is active when the light source trigger is used), or can be read the previously acquired and saved, using the Browse button.

2. Saving Reference and Dark Spectrum
Saving the reference and dark spectrum, they can be used for the subsequent measurement.
SEC2020 Spectrometer is ready to set the target sample for the measurement and for trigger setting.

Trigger setting

For the synchronized measurement with electrochemical measurement, set the trigger mode in the SEC2021 Spectrometer first.

SEC2020 Spectrometer system is ready to receive the output signal from the electrochemical analyzer to start the sysnchronized measurement.

Framework (Interface 1010TM)

Pressing OK, starts the output signal, and the SEC2020 Spectrometer system receives the signal, starting the measurement.
The cyclic voltammetry is saved in the Framework data folder, and the spectrum data can be saved in the specified folder and filename.

Cyclic voltammetry and absorbance spectrum

  
Fig. 24 Cyclic voltammogram and absorbance by synchronizing spectroelectrochemical measurement.
Fig. 24 Cyclic voltammogram and absorbance by synchronizing spectroelectrochemical measurement.