Spooling electrochemiluminescence spectroscopy: development, applications and beyond

Mahdi Hesari, Zhifeng Ding

Published: 2021-03-16 DOI: 10.1038/s41596-020-00486-x

Extended

Extended Data Fig. 1 Assembly of a platinum electrode inside a soft glass.

A vacuum tube is attached to one end of the soft glass to assist with Pt rod insertion into the other end.

Extended Data Fig. 2 Schematic assembly of ECL cell-focus lens-PMT.

A photograph of an exemplary ECL cell including WE (Pt disc), CE (Pt coil), RE (Pt coil), sample solution, quartz window, focus lens, and a PMT along with a recorder. Note that the represented distances are not scaled.

Extended Data Fig. 3 An illustration of optical filter position.

a , Top view of the spectrograph port where a filter is placed to block the excitation light source to perform a spooling photoluminescence spectroscopy. b , Side view of the filter and spectrograph port.

Extended Data Fig. 4 Spooling spectroscopy software setup.

A representative of an Andor iDus camera acquisition setup (red box), acquisition mode, exposure time and kinetic series length (pink boxes) are set as spooling, time interval between each spectrum, and total number of spectra. As a common example, experimental parameters related to spooling ECL spectroscopy of 0.1 mM [Ru(bpy) 3 ](PF 6 ) 2 (Fig. 9 ) in the presence of 5 mM tri- n -propylyamine (TPrA) are displayed. The spooling ECL spectra are shown in Fig. 12a . In this exemplary experiment, the applied potential was scanned from 0.0 V to +1.5 V and back to 0.0 V vs. SCE where TPrA was oxidized at ~0.8 V to produce TPrA radicals. At the close potential, Ru(bpy) 3 2+ lost one electron at ~1.1 to Ru(bpy) 3 3+ . The total time required for the cycle of potential scan is 30 sec. Thus, one can perform a spooling ECL spectroscopy of Ru(bpy) 3 2+ / TPrA by setting up camera acquisition (red box) and selecting “kinetic” for acquisition mode (first pink box at left). Individual spooling spectra can be collected during 1 s of camera exposure time (second pink box at top left). Usually, the number of accumulations needs to be 1. Finally, “kinetic series length” (third pink box at left) represents total time required for an experiment to complete, which is 30 sec in the present example. The spectrum time interval is defined as the density of the collected spectra in time-space. The shorter the time interval, the higher the number of spectra. To set up a trigger, one needs to set the triggering option to “External Start” which means the camera will start to acquire a spectrum (according the setting) as soon as the external signal has been sent through the coaxial cable from the potentiostat.

Extended Data Fig. 5 Spooling spectroscopy software setup.

Before running a spooling spectroscopy experiment, choose the spooling tab (pink tab) in the acquisition setting (red box) and enable spooling. Next, select “Sif” (shown with arrow) as the file type (first green box at top left). One can choose a file name, e.g., “spool” which will be saved with a “.sif” extension. Lastly, select a path where the recorded file will be saved. Note 1: the last two steps can also be done manually. Note 2: all the recorded spooling files with “.sif” extension should be converted to “.acs” in order to be opened with Igor Pro or MATLAB for plotting.

Extended Data Fig. 6 Exemplary electrode junctions.

Photographs of assembled a , counter electrode, and b , reference electrode inside glass capillaries to protect CE and RE from possible side reactions.

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References

One of the most widely used techniques to generate light through an efficient electron transfer is called electrochemiluminescence, or electrogenerated chemiluminescence (ECL). ECL mechanisms can be explored via ‘spooling spectroscopy’ in
Introduction
Materials
Procedure
Troubleshooting
Timing
Anticipated results
- Reporting Summary
- References
References
ACKNOWLEDGMENTS

Hesari, M. & Ding, Z. Review—electrogenerated chemiluminescence: light years ahead. J. Electrochem. Soc. 163, H3116–H3131 (2016).
Zhou, X. et al. Synthesis, labeling and bioanalytical applications of a tris(2,2′-bipyridyl)ruthenium(II)-based electrochemiluminescence probe. Nat. Protoc. 9, 1146–1159 (2014).
Acharya, D. et al. An ultrasensitive electrogenerated chemiluminescence-based immunoassay for specific detection of Zika virus. Sci. Rep. 6, 32227 (2016).
Hesari, M. & Ding, Z. A grand avenue to Au nanocluster electrochemiluminescence. Acc. Chem. Res. 50, 218–230 (2017).
Liu, Z., Qi, W. & Xu, G. Recent advances in electrochemiluminescence. Chem. Soc. Rev. 44, 3117–3142 (2015).
Kalyuzhny, G., Buda, M., McNeill, J., Barbara, P. & Bard, A. J. Stability of thin-film solid-state electroluminescent devices based on tris(2,2‘-bipyridine)ruthenium(II) complexes. J. Am. Chem. Soc. 125, 6272–6283 (2003).
Swanick, K. N., Hesari, M., Workentin, M. S. & Ding, Z. Interrogating near-infrared electrogenerated chemiluminescence of Au25(SC2H4Ph)18+ clusters. J. Am. Chem. Soc. 134, 15205–15208 (2012).
Swanick, K. N., Ladouceur, S., Zysman-Colman, E. & Ding, Z. Self-enhanced electrochemiluminescence of an iridium(III) complex: mechanistic insight. Angew. Chem. Int. Ed. 51, 11079–11082 (2012).
Hesari, M., Ding, Z. & Workentin, M. S. Electrogenerated chemiluminescence of monodisperse Au144(SC2H4Ph)60 clusters. Organometallics 33, 4888–4892 (2014).
Hesari, M., Workentin, M. S. & Ding, Z. Near-infrared electrochemiluminescence from Au25(SC2H4Ph)18+ clusters co-reacted with tri-n-propylamine. RSC Adv 4, 29559–29562 (2014).
Hesari, M., Workentin, M. S. & Ding, Z. Highly efficient electrogenerated chemiluminescence of Au38 nanoclusters. ACS Nano 8, 8543–8553 (2014).
Hesari, M., Workentin, M. S. & Ding, Z. NIR electrochemiluminescence from Au25– nanoclusters facilitated by highly oxidizing and reducing co-reactant radicals. Chem. Sci. 5, 3814–3822 (2014).
Hesari, M., Workentin, M. S. & Ding, Z. Thermodynamic and kinetic origins of Au250 nanocluster electrochemiluminescence. Chem. Eur. J. 20, 15116–15121 (2014).
Yu, Z. et al. High-resolution shortwave infrared imaging of vascular disorders using gold nanoclusters. ACS Nano 14, 4973–4981 (2020).
Ma, W. et al. Investigating electron-transfer processes using a biomimetic hybrid bilayer membrane system. Nat. Protoc. 8, 439–450 (2013).
Gao, R. et al. Wireless nanopore electrodes for analysis of single entities. Nat. Protoc. 14, 2015–2035 (2019).
Ma, W., Ma, H., Peng, Y. Y., Tian, H. & Long, Y. T. An ultrasensitive photoelectrochemical platform for quantifying photoinduced electron-transfer properties of a single entity. Nat. Protoc. 14, 2672–2690 (2019).
Pei, Q., Yu, G., Zhang, C., Yang, Y. & Heeger, A. J. Polymer light-emitting electrochemical cells. Science 269, 1086–1088 (1995).
Chu, K. et al. Electrogenerated chemiluminescence and electroluminescence of n-doped graphene quantum dots fabricated from an electrochemical exfoliation process in nitrogen-containing electrolytes. Chem. Eur. J. 26, 15892–15900 (2020).
Ding, Z. et al. Electrochemistry and electrogenerated chemiluminescence from silicon nanocrystal quantum dots. Science 296, 1293–1297 (2002).
Wong, J. M. et al. Revealing crystallization induced blue shift emission of a di-boron complex by enhanced photoluminescence and electrochemiluminescence. Angew. Chem. Int. Ed. 59, 17461–17466 (2020).
Hesari, M., Lu, J.-s, Wang, S. & Ding, Z. Efficient electrochemiluminescence of a boron-dipyrromethene (BODIPY) dye. Chem. Commun. 51, 1081–1084 (2015).
Hesari, M. et al. Structural tuning of boron difluoride formazanate electrochemiluminescence mediated by tri-n-propylamine. J. Phys. Chem. C 122, 1258–1266 (2018).
Hesari, M., Barbon, S. M., Staroverov, V. N., Ding, Z. & Gilroy, J. B. Efficient electrochemiluminescence of a readily accessible boron difluoride formazanate dye. Chem. Commun. 51, 3766–3769 (2015).
Hercules, D. M. Chemiluminescence resulting from electrochemically generated species. Science 145, 808–809 (1964).
Chandross, E. A. & Sonntag, F. I. A novel chemiluminescent electron-transfer reaction. J. Am. Chem. Soc. 86, 3179–3180 (1964).
Santhanam, K. S. V. & Bard, A. J. Chemiluminescence of electrogenerated 9,10-diphenylanthracene anion radical. J. Am. Chem. Soc. 87, 139–140 (1965).
Collinson, M. M. & Wightman, R. M. Observation of individual chemical reactions in solution. Science 268, 1883–1885 (1995).
Miao, W. Electrogenerated chemiluminescence and its biorelated applications. Chem. Rev. 108, 2506–2553 (2008).
Richter, M. M. Electrochemiluminescence (ECL). Chem. Rev. 104, 3003–3036 (2004).
Ma, C., Cao, Y., Gou, X. & Zhu, J.-J. Recent progress in electrochemiluminescence sensing and imaging. Anal. Chem. 92, 431–454 (2020).
Qi, H. & Zhang, C. Electrogenerated chemiluminescence biosensing. Anal. Chem. 92, 524–534 (2019).
Voci, S. et al. Surface-confined electrochemiluminescence microscopy of cell membranes. J. Am. Chem. Soc. 140, 14753–14760 (2018).
Ouyang, J. & Bard, A. J. Electrogenerated chemiluminescence: Part IL. Emission from acetonitrile solutions containing no added luminescors. J. Electroanal. Chem. 222, 331–342 (1987).
Shen, M. et al. Electrochemistry and electrogenerated chemiluminescence of a novel donor−acceptor FPHSPFN red fluorophore. J. Phys. Chem. C 114, 9772–9780 (2010).
Guo, W. et al. Potential-resolved multicolor electrochemiluminescence for multiplex immunoassay in a single sample. J. Am. Chem. Soc. 140, 15904–15915 (2018).
He, Y., Yang, L., Zhang, F., Zhang, B. & Zou, G. Tunable electron-injection channels of heterostructured ZnSe@CdTe nanocrystals for surface-chemistry-involved electrochemiluminescence. J. Phy. Chem. Lett. 9, 6089–6095 (2018).
Kang, Y. & Kim, J. Electrochemiluminescence of glutathione-stabilized Au nanoclusters fractionated by gel electrophoresis in water. ChemElectroChem 7, 1092–1096 (2020).
Yang, F. et al. 3D matrix-arranged AuAg nanoclusters as electrochemiluminescence emitters for click chemistry-driven signal switch bioanalysis. Anal. Chem. 92, 2566–2572 (2020).
Hesari, M. et al. Highly efficient dual-color electrochemiluminescence from BODIPY-capped PbS nanocrystals. J. Am. Chem. Soc. 137, 11266–11269 (2015).
Hesari, M. et al. Enhancing electrochemiluminescence of chalcogenide clusters by means of Mn replacement. Electrochimica Acta 210, 79–86 (2016).
Maar, R. R. et al. Aluminum complexes of N2O23– formazanate ligands supported by phosphine oxide donors. Inorg. Chem. 56, 12436–12447 (2017).
Kim, J. M., Jeong, S., Song, J. K. & Kim, J. Near-infrared electrochemiluminescence from orange fluorescent Au nanoclusters in water. Chem. Commun. 54, 2838–2841 (2018).
Shu, J. et al. Potential-resolved multicolor electrochemiluminescence of N-(4-aminobutyl)-n-ethylisoluminol/tetra(4-carboxyphenyl)porphyrin/TiO2 nanoluminophores. Anal. Chem. 89, 12636–12640 (2017).
Guo, W., Ding, H. & Su, B. Electrochemiluminescence of metallated porous organic polymers. J. Electroanal. Chem. 818, 176–180 (2018).
Fu, L., Zhang, B., Fu, K., Gao, X. & Zou, G. Electrochemically lighting up luminophores at similar low triggering potentials with mechanistic insights. Anal. Chem. 92, 6144–6149 (2020).
Bard, A. J. & Faulkner, L. R. Electrochemical Methods: Fundamental and Applications 2nd edn (John Wiley & Sons, 2001).
Doeven, E. H. et al. A potential-controlled switch ON/OFF mechanism for selective excitation in mixed electrochemiluminescent systems. Chem. Sci. 4, 977–982 (2013).
Hogan, C. F., Francis, P. S. & Doven, E. H. Multicolour electrochemiluminescence. in Analytical Electrogenerated Chemiluminescence: From Fundamentals to Bioassays (ed. Sojic, N.) 200–246 (Royal Society of Chemistry, 2020).
Climent, V. & Feliu, J. M. Cyclic voltammetry. in Encyclopedia of Interfacial Chemistry. (ed. Wandelt, K.) 48–74 (Elsevier, 2018).

Spooling electrochemiluminescence spectroscopy: development, applications and beyond

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