Experimental Guide for Synchronized Spectroelectrochemical Measurements (Using SEC2020 + Model3325)
Spectroelectrochemical measurements can be understood as the synchronized measurement of spectroscopic changes in a specimen solution near an electrode during an electrochemical reaction. This method can simultaneously obtain information on electrochemical variables (current, charge and potential) and spectroscopic variables (transmittance, absorption, reflection) in the electrode process experiment, which is helpful for further research on the mechanism and intermediate analysis of the electrode process and the characterization of the product.
In general, spectroelectrochemical measurements require the use of a potentiostat and a spectrometer at the same time, but are characterized by the use of a special working electrode, the “transmittance electrode”, and a special measuring cell, the “thin-layer spectroscopic cell”. The spectroelectrochemical synchronization of the measurement is furthermore achieved by triggering the spectrometer (hardware/software) with a potentiostat (hardware/software). In this section, Model 3325 Bi-Pootentiostat and SEC2020 Spectrometer system are used to introduce how to set up the trigger control (hardware/software) to perform the spectroelectrochemical synchonized measurement.
The Model3325 Bi-Potentiostat and SEC2020 Spectrometer system are used here as an example of how to set up the trigger control (hardware/software) to achieve synchronized spectroelectrochemical measurement.
光谱电化学同步测量系统 (SEC2020+Model 3325)
When performing trigger control, the trigger connection line (trigger-input) attached to the SEC2020 spectrometer is controlled and connected with the trigger signal output line (trigger-output) of the Model3325 Bi-Potentiostat to perform the trigger control of the spectrometer (control software) for measurement by the potentiostat (control software) and achieve the synchronization of the two measurements. Trigger control is simply divided into two major components. Hardware settings (trigger control connection between Model3325 and SEC2020 devices), and software settings (trigger signal output of Model3325 software, and trigger signal input setting of SEC2020 software). The above picture shows the connections of the systems after the settings are completed.
Trigger measurement mode
The I/O ports of the SEC2021 spectrometer in the SEC2020 Spectrometer system are equipped with Inpit/Output signal. By connecting the spectrometerto the output ports (#4, #5, #6) to the SEC2022 light source, the SEC2022 light source can be automatically controlled by the control software of the spectrometer (switching on/off of the shutter, deuterium lamp, tungsten-halogen lamp). The “Trigger Input” port (#7) also accepts the “Trigger Output” control signal from an external device (potentiostat) to automatically synchronize the measurement with the external device. For trigger control, simply connect the trigger cable to the corresponding pin to realize various automatic control functions.
- 光谱电化学同步测量系统之硬件构成
- 触发线之连接方法
- 薄层测量池SEC-C
Configuration for Spectroelectrochemical Synchronized Measurement
The electrochemical measurement synchronized with a spectrum monitoring is introduced in this section.
This section will introduce the basic configuration and system settings for synchronzed spectroelectrochemical measurements using the Model 3325 Bi-Potentiostat and the SEC2020 Spectrometer system for spectrum measurements.
光谱电化学同步测量系统的硬件体系，主要由三大部分组成 1）光谱仪(SEC2020)，2）电位仪(Model3325)， 3）光谱电化学反应池（本例中的SEC-C薄层石英玻璃光谱化学电池套件，以及其它配件）。
下面分别介绍这3大组成部分。
1）SEC2020 光谱仪系统(触发指令接受设备，光谱测量）
不同与通常的光谱测量控制，在进行光谱电化学同步测量控制时，光谱仪需要与外部触发控制信号输入线(Signal-in cable)连接，以接受外部设备的触发控制。以下列出了光谱仪系统使用的各个部件。
图1 SEC2020光谱仪系统各组成部件
1) SEC2021光谱仪
1a) 光谱仪入光口保护盖
2) SEC2022 氘卤光源
2a) 光源出光口保护盖
3) 比色皿池座
4) 光纤准直透镜
5) SMA905型遮光螺帽（比色皿池座用 )
6) SEC2024 底座
7) 光源遥控/触发控制一体化连线
2）Model 3325 双恒电位仪 （触发指令输出设备，电化学测量）
使用Model3325双恒电位仪(产品编号013817）进行光谱电化学同步测量控制时，其背面的Cell Control 端口(15针)应与013818 CB-VS远程电缆（15pin)（Signal-output cable)连接，然后再与SEC2020光谱仪的外部触发控制信号输入线进行对接,以实现Model 3325控制软件(产品编号013349）对外部设备（SEC2021光谱仪）控制软件的触发同步测量控制。
图2 Model 3325双恒电位仪
背面接线名称
1) USB线(连接电脑）
2) Cell control端口连接用
013818 CB-VS远程电缆(15pin)
3) 电极线缆接口
3）SEC-C 石英玻璃薄层光谱电化学池套件及附件
图3 SEC-C 石英玻璃薄层光谱电化学池套件和参比电极
各部件名称
013716 SEC-CT 石英玻璃薄层光谱电化学池套件（铂）
(011501) SEC-C 特氟龙池盖
(013718) SEC-CT 石英玻璃薄层光谱电化学池
(011498) SEC-C 铂丝纱网工作电极
(013703) SEC-C /C05用铂对电极
013613 RE-1BP参比电极 (Ag/AgCl)
图4 印刷电极用IC夹
由于SEC-C 铂丝纱网工作电极（011498）铂丝导线的直径为0.5 mm ，因此非常脆弱容易弯曲折。请勿将电位仪的鳄鱼夹直接夹在其上面。
为防止电极损坏，建议使用图4 印刷电极用IC夹进行电极与电位仪之间的连接。
011840 印刷电极用IC夹(4个装）