High Throughput Methodology for Investigating Green Hydrogen Generating Processes using Colorimetric Detection Films and Machine Vision

06 March 2024, Version 1
This content is a preprint and has not undergone peer review at the time of posting.

Abstract

The generation of hydrogen from abundant and renewable precursors driven by sunlight will be a cornerstone of a future, sustainable hydrogen infrastructure. Current methods to monitor the evolution of hydrogen in such photocatalytic systems such as gas chromatography, mass spectrometry, manometry or Raman spectroscopy are either expensive and low throughput or lack sensitivity and selectivity over other gasses. This impediment hinders the generation of photo-driven hydrogen evolution data necessary for machine learning and artificial intelligence-based protocols. This work presents an open-source approach for studying solar-driven hydrogen evolution reactions (HERs) in parallel that uses colorimetric hydrogen detection films in tandem with an image analysis software capable of providing metrics such as hydrogen amount, hydrogen evolution rates, incubation times, and plateau times, and more. The sensing medium is composed of 0.05 % (w/w) Pt impregnated molybdenum (VI) oxide or tungsten (VI) oxide which was incorporated into poly(vinyl alcohol) films placed under clear, gas impermeable septa. To conduct experiments, users require only blue reaction-driving high intensity LEDs, a camera, and uniform lighting to take pictures as the septa darken. This work introduces a sample configuration in which nine samples in hydrogen sensitive septa-capped vials were illuminated and the gas evolution is monitored using a RaspberryPi for image capture and storage. Two calibration methods are presented, one uses a gravimetric hydrogen evolution with Zn/HCl that is compared to a direct hydrogen injection. Both methods allow the accurate correlation of normalized intensity values of film photographs to mole fractions of H2 ranging from 0 to 50%. Four light-driven HERs are described that highlight the capabilities of the detection method, two of which were conducted using the novel septa-based instrumentation while the other two experiments used the films on a 108 multiwell plate using a previously discussed photoreactor.

Keywords

High-Throughput Experimentation
Solar Hydrogen
Colorimetric Hydrogen Detection
Photo Reactor
Data Analysis and Machine Learning

Supplementary materials

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Supporting Information PDF
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PDF File of the Raspberry PI wiring and a calibration graph for the film used on a multi-well plate
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Software for Controlling Photoreactors
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This is a folder that contains all the software to control photo reactors with a Raspberry Pi computer alongside a READ ME and the required libraries
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Image Analysis Software
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This is a folder that contains all the software to analyze the colorimetric responses of the hydrogen films during calibration and experiment
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Sample Holder 3D Printing Files
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All the information to print a sample holder for 9 EPA vials that can be equipped with a hydrogen sensitive film septa
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Experiment 2: Processed Data and Movie
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The folder contains a CSV file with the data analysis created by the image analysis software alongside a movie documenting the darkening of the films covering the 108-well reactor during illumination
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