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electrochemistry experiments

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Practical videos | 16–18 years

  • 1 Access free videos to support your teaching
  • 2 Electrochemical cells
  • 3 Preparation of an organic liquid
  • 4 Rates of reaction
  • 5 Qualitative tests for organic functional groups
  • 6 Titration
  • 7 Thin layer chromatography
  • 8 Reflux and distillation
  • 9 Enthalpy change determination
  • 10 Gravimetric analysis
  • 11 Qualitative tests for anions and cations
  • 12 Rates of hydrolysis

Electrochemical cells

By Tim Jolliff , David Paterson and Sandrine Bouchelkia

  • Five out of five

Investigate electrochemical cells with two microscale experiments

Practical work based on electrochemistry offers opportunities for learners to investigate the thermodynamic feasibility of reactions and apply their knowledge of the reactivity series. 

Source: © Royal Society of Chemistry

Chapter titles: 00:15 Introduction; 01:30 Electrochemical cell set-up (including animation); 02:15 Investigating redox reactions (microscale set-up); 03:23 Taking measurements; 04:09 Animation showing cells in microscale; 06:18 Cell diagrams; 07:43 Investigating concentration.

  • Teacher notes

Full teacher notes are available in the  supporting resources booklet , including ideas for  how to use this video  and the supporting resources as part of your teaching. 

Technician notes including the equipment list and safety notes are provided. If you are planning to carry out the practical in the classroom, you will need to carry out your own risk assessment.

For guidance on how to use this practical with learners aged 14-16, see A micro approach to electrochemical cells yields big learnings .

Prior knowledge 

The video and resources assume the following prior knowledge:

  • Metals can be ordered into a reactivity series.
  • The more reactive metal is a stronger reducing agent.
  • Zinc is more reactive than copper.
  • Oxidation and reduction defined in terms of electron transfer - OIL RIG.
  • Electrons are negatively charged and move from a negative terminal to a positive terminal.
  • ∆G is negative for feasible reactions.

Learners could be directed to our 14–16 video with supporting resources Electrolysis of aqueous solutions , for revision prior to this practical.

Common misconceptions

Be aware of misconceptions learners may have around this practical, for example:

  • Only metals can be placed in the reactivity series.
  • Large quantities of solutions are needed.
  • A sizeable current is flowing when we measure the voltage.
  • How the salt bridge works.
  • Surface area of the metal will change the electrode potential.

This article Redox: reducing difficulties , looks at common misconceptions more closely and suggests strategies to address them.

Further practical activities

The demonstration The oxidation states of vanadium explores different colours of different oxidation states of the transition metals and continues to develop the knowledge that electrode potentials can be used to help predict the course of redox reactions.

Our exhibition chemistry video Nailing corrosion demonstrations looks at rusting from an electrochemical perspective.

Also check out…

  • Explaining electrolytes explicitly – the latest research indicates that students’ grasp of electrolyte chemistry may not be as well developed as we assume.
  • More ideas for teaching in 5 ways to explain electrolysis .
  • Battery power – the perfect resource for when you need an overview of the many different types of batteries and their histories.

Electrochemical cells: supporting resources

Electrochemical cells: technician notes, electrochemical cells: learner notes, electrochemical cells: integrated instructions, additional information.

The original video script and supporting resources were written by Tim Jolliff. The integrated instructions were produced by David Paterson and the technician notes were written by Sandrine Bouchelkia.

The hand of a teacher in a lab coat gestures towards a Liebig condenser used for distillation

Access free videos to support your teaching

A Petri dish set up for a microscale electrolysis experiment using samples of metal and a power supply

Preparation of an organic liquid

A teacher in a lab coat pours a clear liquid into beakers using a measuring flask

Rates of reaction

Test tubes marked A to F in a blue test tube holder; each one contains some clear liquid and is sealed with a bung

Qualitative tests for organic functional groups

Titration

Thin layer chromatography

Image - feature - wooster - fig 5

Reflux and distillation

Maths-a-level-calculationsiStock51914234300tb

Enthalpy change determination

0313EiC_Feature_Spectroscopy_pg23_250

Gravimetric analysis

Copper flame test

Qualitative tests for anions and cations

image - column - reach main 1

Rates of hydrolysis

Chemical reaction-Pipette, producing carbon dioxide

  • 16-18 years
  • Practical experiments
  • Technician notes

Specification

  • 7 Use of appropriate apparatus and techniques to draw, set up and use electrochemical cells for separation and production of elements and compounds
  • j) setting up of electrochemical cells and measuring voltages
  • g) the techniques and procedures used for the measurement of cell potentials of: metals or non-metals in contact with their ions in aqueous solution; ions of the same element in different oxidation states in contact with a Pt electrode
  • set up electrochemical cells and measure voltages
  • (a) redox reactions in terms of electron transfer
  • (b) how to represent redox systems in terms of ion/electron half-equations and as halfcells in cell diagrams
  • (c) concept of standard electrode potential and role of the standard hydrogen electrode
  • (d) how simple electrochemical cells are formed by combining electrodes (metal/metal ion electrodes and electrodes based on different oxidation states of the same element)
  • (e) concept of cell EMF and its significance in terms of the feasibility of reactions
  • PRACTICAL: Construction of electrochemical cells and measurement of Ecell
  • (a) how to construct ion/electron half-equations, for example, for the reduction of acidified Cr₂O₇²⁻ to Cr³⁺ and acidified MnO⁴⁻ to Mn²⁺ and the oxidation of S₂O₃²⁻ to S₄O₆²⁻
  • (b) how to combine half-equations to give a stoichiometric redox equation
  • determine the electrode potentials of a series of cells and predict their values using standard electrode potentials;
  • 5.6.2 use standard electrode potentials to predict feasibility and direction of reactions, to calculate the emf and demonstrate understanding of the limitations of such predictions in terms of concentrations and kinetics.
  • Oxidation and reduction in terms of loss and gain of electrons.
  • Oxidising and reducing agents.
  • The electrochemical series as a series of metals arranged in order of their ability to be oxidised (reactions, other than displacement reactions, not required).
  • Mandatory experiment 1.2 - Redox reactions of group VII elements - halogens as oxidising agents (reactions with bromides, iodides, Fe²⁺ and sulfites). Displacement reactions of metals (Zn with Cu²⁺, Mg with Cu²⁺). (Half equations only required e.g. 2Br⁻…
  • The electrochemical series (reactions of metals with acids, water and oxygen not required).

Related articles

Previews of the Electrochemical cells misconception buster student sheets and teacher notes, and a lemon battery

Electrochemical cells misconception buster | 16–18 years

By Louise Hussein

Probe learners’ knowledge of setting up electrochemical cells, redox equations and calculations

Simple electrolysis experiment set up with power pack and electrodes in beaker of blue solution

Electrolysis – practical videos | 14–16 students

By Karen Marshall , Ian Davies and Sandrine Bouchelkia Five out of five

Video and supporting resources investigating electrolysis of aqueous solutions.

1 Reader's comment

Only registered users can comment on this article., more practical.

A hand is lighting a spirit burner with a match and there is a colourful border around the edge of the image

Enthalpy change of combustion of ethanol | practical videos | 14–16 years

By Karen Marshall and Sandrine Bouchelkia

Video and resources investigating the heat energy change of combustion of ethanol

Simple distillation experiment set up, showing a conical flask containing a black coloured solution sitting on a gauze and tripod over a Bunsen burner. A bung is in the flask and a delivery tube connects it to a test tube in a beaker of ice water

Simple distillation | practical videos | 14–16 years

By Dorothy Warren and Sandrine Bouchelkia

Video and resources showing how to separate water from a coloured solution

Chromatogram sitting in a beaker. The paper has a pencil line with three labels, marked as 1, 2 and 3. Sample 1 has separated into blue, orange and pink up the paper. Sample 2 is still a black circle of ink on the pencil line and sample 3 contains orange

Paper chromatography | practical videos | 14–16 years

Video and resources showing how to separate colours in inks using paper chromatography

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Electrochemical experiments for students

To familiarize students with electrochemical experiments, PalmSens has prepared six theoretical article series with corresponding experiments (in PDF). Each series includes instructional theory to understand the experiment, and the experiment describes a description of the equipment, sensors and chemicals you need.

The experiments

Every experiment has been chosen for its representative character. A particular experiment can serve as an illustration of theoretical aspects or it can be used as a model for electrochemical applications. The goals of each experiment will be given at the beginning of the corresponding experiment’s description. A theoretical introduction and reasons for the outcome will be provided as well.

The experiments are sorted by increasing difficulty. Due to different backgrounds in education, you may want to do the experiments in a different order or perform only selected experiments. Please, feel free to do so. All this material should be considered as a starting point for the lab course or lesson. It most likely needs refinement according to the goals of your lab class and the knowledge the students already have. However, if you feel that this guide could be improved or if you would like to give us feedback, please don’t hesitate to write using https://www.palmsens.com/contact/ .

Here we link to the introductory page of each article series:

  • Copper and Nickel Deposition
  • The Cottrell Experiment and Diffusion Limitation
  • Cyclic Voltammetry – the Most Used Technique
  • Detection of Multiple Heavy Metals by Stripping Voltammetry
  • Detection of Glucose with a Self-Made Biosensor Based on Glucose Oxidase
  • Detection of Hydrogen Peroxide with Selfmade Prussian Blue Electrodes

The equipment and sensors can be bought via the PalmSens store . Please note that teachers can request the answers to the question in the instructions, using https://www.palmsens.com/contact/

  • What are Screen-printed electrodes and which electrode should I choose?
  • Electronic (bio)sensors using FET as the transducer
  • Coulometric Detection
  • Potentiostatic Chronoamperometry
  • Constant Potential Chronoamperometry

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>> Introduction

Electrochemistry: Galvanic Cells and the Nernst Equation

Introduction.

electrochemistry experiments

In this experiment:

  • We will build and investigate several galvanic cells.
  • We will investigate the chemical reactions taking place in various galvanic cells and measure the cell potentials .
  • We will study the electrodes that can be combined in various ways to form many different galvanic cells. We will determine the potential of these cells under standard conditions .
  • We will investigate how the potential of the galvanic cell changes when we depart from the conditions defined as a "standard" and use the Nernst Equation to predict these changes.

electrochemistry experiments

Step 2 Action: Create several half-cells, each consisting of a metal strip (an electrode) dipped in solution of that metal’s salt (an electrode solution). Combine various half-cells into pairs (galvanic cells) and try them out to power a stopwatch. Result: We identify the galvanic cells which provide enough voltage to power a stopwatch.

Step 3 Action: Combine various half-cells into pairs (galvanic cells) and measure the voltage of the various pairs of half-cells. Result: Create a series of electrode potentials arranged in order of the tendency of a metal ion to undergo reduction.

Step 4 Action: We measure voltage of a cell under standard conditions (1.0 M concentration). We change the concentration of one of the half-cells and observe the effect on the cell voltage. We repeat with various half-cell combinations. Result: We determine the values of cell voltage under non-standard conditions.

The following pages contain tutors to assist you with understanding and applying some concepts required in the above steps. Please click next to continue to the online activity.

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Electrochemical Investigations

Author: J. M. McCormick

Last Update: November 28, 201 2

Introduction

In this exercise you will be investigating the potential difference (i. e. voltage) that exists between two pieces of metal when each is placed in a solution containing one of its ions.  In this exercise each group will be assigned one of six metal/ion pairs to investigate.  The metals and ions to be investigated are Al/Al 3+ , Cu/Cu 2+ , Ni/Ni 2+ , Pb/Pb 2+ , Fe/Fe 3+ and Zn/Zn 2+ .  You will first examine the effect of concentration by changing the concentration of metal ion solution outside the porous cup and derive an empirical equation that describes this effect.  You will then investigate the effect of addition of OH – to the metal ion solution outside the cup.  Finally, you will investigate what happens when you have one metal and its salt coupled to a different metal and its salt with all of the salt solutions at the same concentration.

Figure 1. Schematic of the experimental apparatus used in this exercise.

The experimental set-up, shown schematically in Fig. 1, consists of a metal electrode immersed in a 0.100 M solution of one of its salts inside a porous porcelain cup. This is the cell’s reference compartment.  The other metal electrode is immersed in a solution of one of its salts.  This is the measurement compartment. The concentration of the salt solution in the measurement compartment does not need to be 0.100 M in the metal ion of interest, but the total salt concentration must be at a relatively high level to be able to make a measurement.  So, another, inert salt is added as a supporting electrolyte to facilitate the measurement.  In this experiment, we will use KNO 3 as the supporting electrolyte. For most of this exercise the two electrodes will be of the same metal, but they are not required to be.

For this exercise, you will be working with your benchmates in a group of four.  One person will check out from the Stockroom two electrodes, a porcelain cup, and four 100 mL beakers for the bench. Be sure to record the metal (i. e., the electrode material) that you are assigned and the salt that you will use in your laboratory notebook. It is important that the salt’s cation be the same element as the electrode. Otherwise, your data will be meaningless.

CAUTION! All of the metals used in this exercise and their salts are toxic (especially Pb) and care must be taken when handling them.  You are advised to wear gloves when handling the electrodes, the solutions and the porcelain cups.  Remove your gloves before handling the digital voltmeter or before using a computer to prevent cross contamination.  Be frugal in your use of the metal ion solutions; they are expensive both in terms of their procurement cost and their disposal cost .  You should not need more than about 60 mL of the 0.100 M solution, and even less of the concentrated solution, for the entire exercise.

Remove the two electrodes from their protective bag. Take care with the electrodes, some of the metals are very soft (Pb) and some of the electrodes may be very thin (Cu, Ni). Add approximately 80 mL of 0.1 M HCl to one of the 100 mL beakers.  Dip the electrodes in the solution and gently  swish them around. It is not necessary to leave them in the solution very long (some will react with the acid).  We only want to remove any oxide coating or other contaminants on the surface.  Rinse the electrodes with a copious amount of distilled water and pat try with a paper towel.

Lightly buff the surface of the electrodes with a piece of fine steel wool.  This will remove the outer layer of metal oxide that coats most metals and any contaminants on the surface, which can interfere with the potential measurements. Do not buff so hard that you remove large amounts of metal.  Again rinse the electrode with distilled water and pat the surface dry with a paper towel to remove any metal or metal oxide dust.

electrochemistry experiments

Figure 2. The Fluke 75 digital voltmeter used in this exercise to measure the potential.

Solution Preparation

A 0.10 M solution and a concentrated solution of each metal salt will be provided. The concentrated solution will be between 0.20 and 0.50 M, depending on the salt’s solubility. Be sure to record the actual concentration of the salt in the concentrated solution in your notebook and adjust your dilutions accordingly. Both of these solutions also contain KNO 3 so that the total concentration of the ions in the solution is 1.0 M, because it is important to maintain a high salt concentration when performing electrochemistry.  Therefore when you perform the dilutions described below, you must use the provided 1.0 M KNO 3 solution and not plain water.

Between you and your bench mates, you will have six 100-mL beakers (if you don’t, your instructor will advise you on how to proceed, although just washing a beaker after you have made a measurement is a simple and efficient option). Label the beakers as follows (assuming your most concentrated solution is 0.50 M; if your most concentrated solution is not 0.50 M, you will need to substitute your actual concentrations for the last two solutions): 0.0040 M, 0.010 M, 0.050 M, 0.10 M, 0.25 M and 0.50 M. Pour 50 mL of the 0.10 M solution into the beaker labeled 0.10 M and 50 mL of your 0.50 M solution (or whatever its concentration is) into its beaker. The other solutions you will prepare by dilution from either the 0.10 M solution (i. e., the 0.004 M, 0.010 M and 0.050 M solutions) or from the 0.50 M solution (i. e., the 0.25 M solution) using your 10-mL and 40-mL graduated cylinders to prepare 50 mL of each of the new solutions.  We will assume that the solution volumes are additive and so mixing 10 mL of the 0.10 M solution with 40 mL of the 1 M KNO 3 solution would give 50 mL of a 0.020 M solution. IMPORTANT! You MUST use the 1 M KNO 3 solution when preparing these dilutions, otherwise your results will be meaningless! Helpful hint: you can help keep down lab costs by waiting to make the 0.25 M solution until after you have made your measurement on the 0.50 M solution.  In this way you can use the 0.50 M solution to make the more dilute solution and not waste valuable reagents.

It may be helpful to use a table, such as Table 1, below to organize your results, where you will replace the actual salt solution concentrations with the suggested values given in Table 1. Be sure to calculate the exact concentration that you used based on the volumes that you actually used. For example, if you took 9.9 mL of the 0.10 M solution and diluted it with 42.0 mL of 1 M KNO 3 , the actual concentration that you would have would be 0.019 M, not 0.020 M.

Concentration (M)Potential (V)
0.0040
0.010
0.050
0.1
0.25
0.50

Table 1. Suggested table for organizing the potential as a function of concentration data in the laboratory notebook.

If time permits, and your instructor allows it, you can prepare and test other concentrations between 0.001 M and 0.5 M.

Cell Set-Up

Place approximately 10 – 15 mL of the 0.1 M salt solution that matches the metal that you have been assigned in the porcelain cup.  The porcelain cups are labeled for each metal; be sure to only use the cup labeled for your metal and do not mix the cups up.  IMPORTANT! Take care handling the porcelain cups; they are fragile and expensive!  You want the level of the solution in the porcelain cup to be at about the same level as the solution in the beaker when you place the porcelain cup into the solutions you just prepared.  This does not have to be exactly the same, but a disparity in liquid levels may cause a systematic error in your results.

Place one of the metal electrodes into the cup; this is your reference compartment.  Place your reference compartment in a beaker ( not one of the 100-mL beakers) until you are ready to use it.  Be aware that the cup is porous and so the solution will drain out if it is left sitting around for any length of time.

Investigation of Concentration’s Effect on Potential

Assemble the cell as shown in Fig. 3 using the 100 mL beaker containing your 0.10 M salt solution.  An iron ring is used to keep the beaker from moving during the measurement (a large three-pronged clamp would work as well), and a clamp is used to position the DVM leads so that the metal electrodes and the metal parts of the leads are not touching each other during the measurement.  Note that you should not actually clamp the leads! Rather, use the clamp to position the electrodes in the proper location.

electrochemistry experiments

Figure 3. The electrochemical cell used in this exercise: the complete set-up is shown on the left and a close-up of the cell showing the reference compartment (a metal electrode immersed in a 0.100 M salt solution of that metal contained in a porous porcelain cup) and the measurement compartment (the beaker with a metal electrode immersed in a solution containing a salt of that metal).

Carefully attach the DVM leads to the electrodes so that the red lead is attached to the electrode in the reference compartment (the porcelain cup) and the black lead is attached to the other electrode.  It is critical that the red lead always be attached to the electrode in the reference compartment and that the electrode and the porcelain cup of the reference compartment do not touch each other. Once you are assured that everything is set up properly, measure the voltage. It may take up to 30 sec for the voltmeter to give a stable reading and you may need to gently stir the outer solution by carefully using the electrode as a stirrer. Record the concentration and voltage reading in your notebook.

Once you have obtained a measurement, shut off the voltmeter and remove the reference compartment and carefully blot away any solution adhering to the outside of the cup with a paper towel. Place the reference in its storage beaker. Remove the second electrode from the cell, rinse with a small amount of distilled water and pat dry with a Kim-Wipe or a paper towel.

Now remove the beaker containing the 0.10 M solution and replace it with the beaker containing the 0.050 M solution. Place the reference compartment and the second electrode into the beaker and attach the leads (be sure that the red DVM lead is attached to the reference compartment’s electrode). Follow the procedure given above to measure the potential for the cell with this solution in the outer compartment, and then repeat for the more dilute solutions and finally for the more concentrated solutions.

What happens to the measured potential as the concentration is lowered? What happens  when the concentration in the outer compartment is greater than the concentration in the reference compartment? Compare your results with other groups; do they see the same thing?

Investigation into the Effect of Adding OH –

To the beaker containing the 0.10 M salt solution, add 5.0 mL of 1.0 M of the provided strong base (either KOH or NaOH) using your 10-mL graduated cylinder and mix well. What do you observe when the base was added?

After a couple of minutes, measure the potential between this solution and your reference compartment.  What do you conclude about the concentration of your metal ion in the solution to which you added the base?

What happens both to the solution and the potential when a second 5.0-mL aliquot of base is added?  What about a third 5.0-mL aliquot?

Investigation into the Effect of the Metal on Potential

In this section you will work with each of the other groups.  Your instructor will designate up to three groups to prepare the cell for this portion of the exercise.  Each of these groups will place their reference cell in a 100 mL beaker containing 50 mL 1 M KNO 3 .  Other groups will place their reference electrode into the beaker to make the measurement and then change to another cell.  Groups will continue to rotate until every possible combination of the electrodes has been measured (see Table 2). When moving a reference compartment, do so in a beaker and use extreme caution. If you are careful, every group should be able to test its electrode with every other electrode, and use no more than 150 mL of the 1 M KNO 3 .

You can use Table 2 as a way to organize your data for these measurements. The Xs in the table indicate measurements that you do not need to make, either because you made them already (e. g., red probe on a Cu electrode in a 0.10 M Cu 2+ solution and the black probe on a Cu electrode in a 0.10 M Cu 2+ solution) or because they are related to another measurement in the table (you can try a few to see what this relationship is). Be sure to include the sign on the potential (some may be negative!).

Black Probe onCuPbNiFeAlZn
X
XX
XXX
XXXX
XXXXX
XXXXxX

Table 2. Summary table for the effect of the metals in an electrochemical cell have on the potential.

Place the metal-containing solutions that you used in the measurements in the appropriate waste bottle that your instructor will show you.

Rinse the electrodes with distilled water and dry with a paper towel or Kimwipe before returning them to the storage package. The porcelain cups should be rinsed with distilled water and the exterior should be gently patted dry with a paper towel.

Return all checked-out materials to the Stockroom.

Results and Analysis

Find a method of graphing the potential as a function of concentration that gives a straight line (helpful hint: you might try graphing potential as a function of a power of the concentration, or as a function of an exponential of the concentration, or as a function of the logarithm of the concentration, or as a function of concentration divided by the concentration in the reference compartment).  Be sure to follow the guidelines described on the Preparing Graphs page when you prepare these graphs.  Note that there may be deviations from linearity at the very lowest and very highest concentrations.

Determine the slope and intercept of your line and compare it to the other groups.  Are the slopes and intercepts the same for all of the groups (remember each group is working with a different metal)? Is there any evidence for a junction potential (i. e., a potential that can result when two solutions are in contact with each other)? Think about how a junction potential would affect the measured potential and where it would be the most evident on your graph.  Do any differences in the slope suggest that is additional information that could be extracted from the data? How might you use a graph to extract this information?

Can you use your potential data from when OH – was added to a solution of your metal to determine the K sp of the metal hydroxide?  If so, determine it and estimate its uncertainty. If not, what additional information, if any, would you need? Share your results with other groups and compare.

From your data where you compared the different metals, the potential (and its sign) depends  on which metals are paired in the electrochemical cell. Rank the metals in an order that reflects your results and compare it to the table of standard reduction potentials found in most general chemistry texts. FYI: it is the convention in electrochemistry to define the direction of spontaneous change ( D G < 0) as having a positive cell potential.

Conclusions

This experiment is a measurement exercise and your discussion should address the points contained in this outline, as well as the questions raised in the Results and Analysis section above.

  • Contents >

Lab 13 - Electrochemistry and the Nernst Equation

Print

Goal and Overview

Objectives and science skills.

  • • Understand and explain the chemistry, components, function, and operation of electrochemical and concentration cells.
  • • Construct electrochemical cells and measure E 0 cell for different pairs of metals and metal ion solutions; identify anode and cathode and explain what occurs at each (oxidation or reduction).
  • • Construct concentration cells and measure E cell values; use experimental values to calculate K sp for slightly soluble silver halide salts.
  • • Quantitatively and qualitatively compare experimental results with theoretical values.
  • • Identify and discuss factors or effects that may contribute to the uncertainties in values determined from experimental data.

Suggested review and external reading

  • • relevant reference information and/or textbook information on thermodynamics, electrochemistry, equilibrium, and free energy

Figure 1

coulomb
mole e
Joule
mole − volt
RT
nF
(0.0591 volts)
n

Part 1: Determinations of E ° for Metals vs. Copper

[A ]
[B ]

To create a voltaic cell:

To create the salt bridge:, part 2: dependence of e on ion concentrations.

Ag
Ag
  • • In cell 1, ions accept electrons from the metal, plate out on the electrode, and lower the concentration of the ions.
  • • In cell 2, atoms in the metal leave electrons behind and enter the solution, thus raising the ion concentration.
  • • The reaction occurs in such a direction as to equalize the concentrations of the two solutions.
E =
(0.0591 V)
n

Figure 2

Part 3: Determination of K sp of Very Insoluble Silver Halides

  • E measured for various metals relative to Cu (i.e. Cu__M 1 ),
  • E °(cell) predicted using metals other than copper
  • c 1 (0.10 M), c 2 , E measured , and log( c 2 / c 1 )
  • graph E versus log ( c 2 / c 1 ), and determine the slope
  • E measured , c Ag + , K sp for AgCl, AgBr, AgI, and Δ G °

Sample Calculations

  • Part 1. Predicted E ° for cells with metals vs. Cu
  • Part 2. log( c 2 / c 1 ) if done
  • Part 3. [Ag + ], K sp (AgCl), Δ G °(AgCl solubility), K sp (AgBr), Δ G °(AgBr solubility), K sp (AgI), Δ G °(AgI solubility)

Discussion/Conclusions

  • Part 1: Does E measured agree with E predicted for the various metals?
  • Part 2: Does the slope agree with the slope predicted by the Nernst equation?
  • Even though cell potentials are affected by both concentration differences and voltage differences between different metals, you were able to determine the dependence on each factor ( RT / nF and E 1/2 °). How were the individual dependencies separated out and determined individually?
  • Part 3: How does part 3 depend on part 2?

Copyright © 2011 Advanced Instructional Systems, Inc. and the University of California, Santa Cruz | Credits

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Two, Three and Four Electrode Experiments

The number of electrodes (or probes) used two, three, four electrode., introduction.

Electrochemical experiments range from simple potentiostatic (chronoamperometry), to cyclic voltammetry (potentiodynamic), to complex AC techniques such as impedance spectroscopy. Moreover, each individual technique may have multiple possible experimental setups, often with a best option. This note discusses one aspect of these setups: the number of electrodes (or probes) used.

Potentiostat as a Four-Probe Instrument

Gamry potentiostats (and some others) are all 4-probe instruments. This means that there are four relevant leads that need to be placed in any given experiment. Two of these leads—Working (green) and Counter (red)—carry the current, and the other two—Working Sense (blue) and Reference (white)—are sense leads which measure voltage (potential).

Color coded leads

Figure 1: Gamry color-coded leads.

Four-probe instruments can be setup to run 2, 3 , or 4 electrode measurements with just a simple change  in setup. Understanding why and how to use the different modes thus is important.

The discussion of n -electrode mode experiments needs to address what the electrodes are. An electrode is a (semi-)conductive solid that interfaces with a(n) (electrolyte) solution. The common designations are: Working, Reference and Counter (or Auxiliary).

Working electrode is the designation for the electrode being studied. In corrosion experiments, this is probably the material that is corroding. In physical-electrochemistry experiments, this is most often an inert material—commonly gold, platinum or carbon—which passes current to other species without being affected by that current. 

The Counter or Auxiliary electrode is the electrode in the cell that completes the current path. All electrochemistry experiments (with non-zero current) must have a working–counter pair. In most experiments the Counter is the current source/sink and so relatively inert materials like graphite or platinum are ideal, though not necessary. In some experiments the counter electrode is part of the study, so the material composition and setup vary accordingly.

Reference electrodes are, as their name suggests, electrodes that serve as experimental reference points. Specifically, they are a reference for the potential (sense) measurements. Reference electrodes should, therefore, hold a constant potential during testing, ideally on an absolute scale. This is accomplished by first having little or, ideally, no current flow through them, and second by being “well-poised,” which means that even if some current does flow it does not affect the potential. While many electrodes could be well-poised, there are several that are very commonly used and commercially available: silver/silver chloride, saturated calomel, mercury/mercury (mercurous) oxide, mercury/mercury sulfate, copper/copper sulfate, and more. There are other couples that are often referenced but are not typically used today, such as the normal hydrogen electrode.

Any conductive material can be used as a reference electrode, but if potential measurements are to be reported that need to be compared with other systems, use of a non-standard reference requires additional experimentation and explanation.

Two-Electrode Experiments

Two-electrode experiments are the simplest cell setups, but often have far more complex results, and corresponding analysis.  In a two-electrode setup the current-carrying electrodes are also used for sense measurement.

The physical setup for two-electrode mode has the current and sense leads connected together: Working (W) and Working Sense (WS) are connected to a (working) electrode and Reference (R) and Counter (C) are connected to a second (aux, counter, or quasi-/pseudo-reference) electrode. See Figure 2 for a diagram of a 2-electrode cell setup.

2-electrode cell setup

Figure 2:  Two-electrode cell setup

Two-electrode experiments measure the whole cell, that is, the sense leads measure the complete voltage dropped by the current across the whole electrochemical cell: working electrode, electrolyte, and counter electrode. If a map of the whole-cell potential looks like Figure 3, then a 2-electrode setup has the Working Sense lead at point A and the Reference lead at point E, and so measures the voltage drop across the whole cell. 

electrochemical cell: working electrode, electrolyte, and counter electrode

Figure 3: Measured (sample) potential map across a whole cell. The Working lead is at point A and the Counter lead is at point E.

Two-electrode setups are used in a couple of general cases. One is where measurement of the whole cell voltage is significant, for example electrochemical-energy devices (e.g., batteries, fuel cells, supercapacitors). The other is where the counter-electrode potential can be expected not to drift over the course of the experiment. This is generally in systems which exhibit very low currents or relatively short timescales and which also have a well-poised counter, e.g., a micro working electrode and a much larger silver counter electrode.

Three-Electrode Experiments

In three electrode mode, the Reference lead is separated from the Counter and connected to a third electrode. This electrode is most often positioned so that it is measuring a point very close to the working electrode (which has both Working and Working Sense leads attached: see Figure 4).

Measured (sample) potential map across a whole cell. The Working lead is at point A and the Counter lead is at point E

Figure 4: 3-electrode cell setup

In Figure 3 the sense points are located at A and—roughly—B. Three-electrode setups have a distinct experimental advantage over two-electrode setups: they measure only one half of the cell. That is, the potential changes of the working electrode are measured independent of changes that may occur at the counter electrode. 

This isolation allows for a specific reaction to be studied with confidence and accuracy. For this reason, 3-electrode mode is the most common setup used in electrochemical experimentation.

There is a second case of the three-electrode setup worth explaining. The Interface 5000 potentiostat can measure the voltage difference between the counter sense and reference for some experiments while simultaneously measuring the voltage difference between the reference and working sense. In this instance, you would connect the counter and counter sense to the counter electrode, the reference to the reference electrode, and the working and working sense to the working electrode. In this particular setup you get both half cells in addition to the full cell in a single experiment.

Four-Electrode Experiments

In four-electrode mode the Working Sense lead is decoupled from the working electrode, as was (and in addition to) the Reference lead (see Figure 5). 

Four-electrode setups measure potential along the B-D line in Figure 3, where there may be some “obstruction” at C. This setup is relatively uncommon in electrochemistry, though it does have its place. In 4-electrode mode, the potentials for any electrochemical reactions that are occurring at the working (and counter) electrode(s) are not being measured. What is being measured is the effect of an applied current on the solution itself or some barrier in that solution.

3-electrode cell setup

Figure 5 : 4-electrode cell setup

The most common use of this setup is to measure impedance across some solution-phase interface, such as a membrane or liquid-liquid junction. This setup can be used to make very accurate measures of solution resistance or the resistance across the surface of some material (solid-state cells). 

Special Case Setup: ZRA Mode

Zero Resistance Ammeter (ZRA) experiments are a special instance. In ZRA mode, the Working and Counter electrode leads are shorted together inside the instrument, i.e., there is zero net voltage dropped across the whole cell. For Gamry instruments, the setup is similar to the 3-electrode setup (Figure 4), with an extra, orange Counter Sense (CS) lead connected to the counter (see Figure 1). The Reference electrode is not critical in this experiment, but can act as a “spectator” electrode to the Working-Counter coupling.

Zero Resistance Ammeter

Figure 6: Measured potential map across a ZRA mode Cell. W/WS at A, C/CS at E. Note that this is not an accurate potential map within the Helmholtz layers. B and D represent closest measurable approaches.

ZRA mode redraws Figure 3 as Figure 6. Now the potential at A equals the potential at E. The reference could be at position B, C, or D. The Reference in solution picks up slightly different potentials based on position, current-flow and solution-resistance.

ZRA mode is used for galvanic corrosion, electrochemical noise, and a handful of specialized experiments.

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Experimental electrochemistry : a laboratory textbook

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  • Preface. Foreword. Symbols and Acronyms. 1 Introduction - An Overview of Practical Electrochemistry. Practical Hints. Electrodes. Measuring Instruments. Electrochemical Cells. Data Recording. 2 Electrochemistry in Equilibrium. Experiment 2
  • .1: The Electrochemical Series. Experiment 2
  • .2: Standard Electrode Potentials and the Mean Activity Coefficient. Experiment 2
  • .3: pH-Measurements and Potentiometrically Indicated Titrations. Experiment 2
  • .4: Redox Titrations (Cerimetry). Experiment 2
  • .5: Differential Potentiometric Titration. Experiment 2
  • .6: Potentiometric Measurement of the Kinetics of the Oxidation of Oxalic Acid. Experiment 2
  • .7: Polarization and Decomposition Voltage. 3 Electrochemistry with Flowing Current. Experiment 3
  • .1: Ion Movement in an Electric Field. Experiment 3
  • .2: Paper Electrophoresis. Experiment 3
  • .3: Charge Transport in Electrolyte Solution. Experiment 3
  • .4: Conductance Titration. Experiment 3
  • .5: Chemical Constitution and Electrolytic Conductance. Experiment 3
  • .6: Faraday's Law. Experiment 3
  • .7: Kinetics of Ester Saponification. Experiment 3
  • .8: Movement of Ions and Hittorf Transport Number. Experiment 3
  • .9: Polarographic Investigation of the Electroreduction of Formaldehyde. Experiment 3
  • .10: Galvanostatic Measurement. Experiment 3
  • .11: Cyclic Voltammetry. Experiment 3
  • .12: Slow Scan Cyclic Voltammetry. Experiment 3
  • .13: Kinetic Investigations with Cyclic Voltammetry. Experiment 3
  • .14: Numerical Simulation of Cyclic Voltammograms. Experiment 3
  • .15: Cyclic Voltammetry with Microelectrodes. Experiment 3
  • .16: Cyclic Voltammetry of Organic Molecules. Experiment 3
  • .17: Cyclic Voltammetry in Nonaqueous Solutions. Experiment 3
  • .18: Cyclic Voltammetry with Sequential Electrode Processes. Experiment 3
  • .19: Cyclic Voltammetry of Aromatic Hydrocarbons. Experiment 3
  • .20: Cyclic Voltammetry of Aniline and Polyaniline. Experiment 3
  • .21: Galvanostatic Step Measurements. Experiment 3
  • .22: Chronoamperometry. Experiment 3
  • .23: Chronocoulometry. Experiment 3
  • .24: Rotating Disc Electrode. Experiment 3
  • .25: Rotating Ring-Disc Electrode. Experiment 3
  • .26: Measurement of Electrode Impedances. Experiment 3
  • .27: Corrosion Cells. Experiment 3
  • .28: Aeration Cell. Experiment 3.29 Concentration Cell. Experiment 3.30 Salt Water Drop Experiment According to Evans. Experiment 3
  • .31: Passivation and Activation of an Iron Surface. Experiment 3
  • .32: Cyclic Voltammetry with Corroding Electrodes. Experiment 3
  • .33: Oscillating Reactions. 4 Analytical Electrochemistry. Experiment 4
  • .1: Ion-sensitive Electrode. Experiment 4.2 Potentiometrically Indicated Titrations. Experiment 4.3 Bipotentiometrically Indicated Titration. Experiment 4.4 Conductometrically Indicated Titration. Experiment 4.5 Electrogravimetry. Experiment 4.6 Coulometric Titration. Experiment 4.7 Amperometry. Experiment 4.8 Polarography (Fundamentals). Experiment 4.9 Polarography (Advanced Methods). Experiment 4.10 Anodic Stripping Voltammetry. Experiment 4.11 Abrasive Stripping Voltammetry. Experiment 4.12 Polarographic Analysis of Anions. Experiment 4.13 Tensammetry. 5 Non-Traditional Electrochemistry. Experiment 5.1 UV-Vis Spectroscopy. Experiment 5.2 Surface Enhanced Raman Spectroscopy. Experiment 5.3 Infrared Spectroelectrochemistry. Experiment 5.4 Electrochromism. 6 Electrochemical Energy Conversion and Storage. Experiment 6.1 Lead Acid Accumulator. Experiment 6.2 Discharge Behavior of Nickel-Cadmium Accumulators. Experiment 6.3 Performance Data of a Fuel Cell. 7 Electrochemical Production. Experiment 7.1 Cementation Reaction. Experiment 7.2 Galvanic Copper Deposition. Experiment 7.3 Electrochemical Oxidation of Aluminum. Experiment 7.4 Kolbe Electrolysis of Acetic Acid. Experiment 7.5 Electrolysis of Acetyl Acetone. Experiment 7.6 Anodic Oxidation of Malonic Acid Diethylester. Experiment 7.7 Indirect Anodic Dimerization of Acetoacetic Ester (3-oxo-butyric acid ethyl ester). Experiment 7.8 Electrochemical Bromination of Acetone. Experiment 7.9 Electrochemical Iodination of Ethano. Experiment 7.10 Electrochemical Production. Experiment 7.11 Yield of Chlor-alkali Electrolysis According to the Diaphragm Process. Appendix. Index.
  • (source: Nielsen Book Data)

Physical Chemistry Chemical Physics

An experimental perspective on nanoparticle electrochemistry.

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* Corresponding authors

a Department of Physics, Technical University of Denmark, 2800 Kongens Lyngby, Denmark E-mail: [email protected]

b Center for Visualizing Catalytic Processes (VISION), Department of Physics, Technical University of Denmark, 2800 Kongens Lyngby, Denmark

c National Centre for Nano Fabrication and Characterization, Technical University of Denmark, 2800 Kongens Lyngby, Denmark

While model studies with small nanoparticles offer a bridge between applied experiments and theoretical calculations, the intricacies of working with well-defined nanoparticles in electrochemistry pose challenges for experimental researchers. This perspective dives into nanoparticle electrochemistry, provides experimental insights to uncover their intrinsic catalytic activity and draws conclusions about the effects of altering their size, composition, or loading. Our goal is to help uncover unexpected contamination sources and establish a robust experimental methodology, which eliminates external parameters that can overshadow the intrinsic activity of the nanoparticles. Additionally, we explore the experimental difficulties that can be encountered, such as stability issues, and offer strategies to mitigate their impact. From support preparation to electrocatalytic tests, we guide the reader through the entire process, shedding light on potential challenges and crucial experimental details when working with these complex systems.

Graphical abstract: An experimental perspective on nanoparticle electrochemistry

  • This article is part of the themed collections: 2024 PCCP Reviews and Size effects in chemistry & physics of atomic & molecular clusters, nanoparticles & nanostructures

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E. Sedano Varo, R. E. Tankard, J. L. Needham, E. Gioria, F. Romeggio, I. Chorkendorff, C. D. Damsgaard and J. Kibsgaard, Phys. Chem. Chem. Phys. , 2024,  26 , 17456 DOI: 10.1039/D4CP00889H

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  • Published: 26 June 2024

Parallel experiments in electrochemical CO 2 reduction enabled by standardized analytics

  • Alessandro Senocrate   ORCID: orcid.org/0000-0002-0952-0948 1 , 2 ,
  • Francesco Bernasconi   ORCID: orcid.org/0000-0002-6563-0578 1 , 3 ,
  • Peter Kraus   ORCID: orcid.org/0000-0002-4359-5003 1 ,
  • Nukorn Plainpan 1 ,
  • Jens Trafkowski 4 ,
  • Fabian Tolle   ORCID: orcid.org/0000-0002-4221-0167 4 ,
  • Thomas Weber 4 ,
  • Ulrich Sauter   ORCID: orcid.org/0009-0000-7623-8697 1 &
  • Corsin Battaglia 1 , 2 , 3 , 5  

Nature Catalysis volume  7 ,  pages 742–752 ( 2024 ) Cite this article

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Electrochemical CO 2 reduction (eCO 2 R) is a promising strategy to transform detrimental CO 2 emissions into sustainable fuels and chemicals. Key requirements for advancing this field are the development of analytical systems and of methods that are able to accurately and reproducibly assess the performance of catalysts, electrodes and electrolysers. Here we present a comprehensive analytical system for eCO 2 R based on commercial hardware, which captures data for >20 gas and liquid products with <5 min time resolution by chromatography, tracks gas flow rates, monitors electrolyser temperatures and flow pressures, and records electrolyser resistances and electrode surface areas. To complement the hardware, we develop an open-source software that automatically parses, aligns in time and post-processes the heterogeneous data, yielding quantities such as Faradaic efficiencies and corrected voltages. We showcase the system’s capabilities by performing measurements and data analysis on eight parallel electrolyser cells simultaneously.

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Data availability.

Data used in this manuscript are freely available via Zenodo at https://doi.org/10.5281/zenodo.8319625 (ref. 54 ). Data for composing Fig. 3 are also part of an interactive example of automated data parsing and processing that can be accessed via Zenodo at https://doi.org/10.5281/zenodo.7941528 (ref. 32 ).

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The code used in this work is fully open source and available at https://dgbowl.github.io/ (ref. 33 ).

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Acknowledgements

This work has received funding from the ETH Board in the framework of the Joint Strategic Initiative ‘Synthetic Fuels from Renewable Resources’. This work was also supported by the NCCR Catalysis, a National Centre of Competence in Research funded by the Swiss National Science Foundation (grant no. 180544). We further acknowledge support by the Open Research Data Program of the ETH Board (project ‘PREMISE’: Open and Reproducible Materials Science Research). A.S. acknowledges funding from the Swiss National Science Foundation through the Ambizione grant PZ00P2_215992. We thank C. Spitz, S. Holmann and M. Maier from Agilent Technologies (Switzerland) for support with validating the chromatographic method. We thank N. Vetsch for help in coding the electrochemical data parser, and J. Viloria for support during electrochemical experiments. E. Querel is acknowledged for help with the ICP measurements. We also acknowledge the support of the Scientific Center for Optical and Electron Microscopy (ScopeM) of the ETH Zurich and of P. Zeng of ScopeM for the focused ion beam-SEM results. We also thank M. Mirolo of beamline ID31 at the European Synchrotron Radiation Facility (ESRF) for support with the synchrotron X-ray measurements.

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A.S. designed, validated and assembled the hardware, performed the main electrochemical experiments and wrote the manuscript with input from all co-authors. F.B. contributed to the electrochemical experiments, validation of the method, assembly of the hardware and acquisition of the SEM images. P.K. wrote the open-source software and contributed to the data analysis. N.P. supported the data analysis effort and wrote the script required to analyse data from parallel cells. J.T., F.T. and T.W. supported the implementation of the online liquid sampling and liquid analysis. U.S. helped writing and debugging the open-source software. C.B. supervised the development of the project.

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Correspondence to Alessandro Senocrate .

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Senocrate, A., Bernasconi, F., Kraus, P. et al. Parallel experiments in electrochemical CO 2 reduction enabled by standardized analytics. Nat Catal 7 , 742–752 (2024). https://doi.org/10.1038/s41929-024-01172-x

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electrochemistry experiments

Left: a molecule schematic of trilayer graphene exchanging an electron with a redox couple of ruthenium hexamine. Center: Line graph with red line with low values at either end of the spectrum and a large peak in the center, blue with more moderate but consistent peaks. Right: Two hexagonal patterns of blue, orange and yellow, one with a repeating color pattern and one with no pattern

Stacking three layers of graphene with a twist speeds up electrochemical reactions

Tri-layer may be better than bi-layer for manufacturing, improving the speed and capacity of electrochemical and electrocatalytic devices

Michigan Aerospace Engineering

Expert‘s name

electrochemistry experiments

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Tri-layer may be better than bi-layer for manufacturing, improving the speed and capacity of electrochemical and electrocatalytic devices Three layers of graphene, in a twisted stack, benefit from a similar high conductivity to”magic angle” bilayer graphene but with easier manufacturing—and faster electron transfer. The finding could improve nano electrochemical devices or electrocatalysts to advance energy storage or conversion.

Graphene—a single layer of carbon atoms arranged in a hexagonal lattice—holds unique properties, including high surface area, excellent electrical conductivity, mechanical strength and flexibility, that make this 2D material a strong candidate for increasing the speed and capacity of energy storage.

Twisting two sheets of graphene at a 1.1° angle, dubbed the “magic angle”, creates a “flat band” structure, meaning the electrons across a range of momentum values all have roughly the same energy. Because of this, there is a huge peak in the density of states, or the available energy levels for electrons to occupy, at the energy level of the flat band which enhances electrical conductivity.

Recent work experimentally confirmed these flat bands can be harnessed to increase the charge transfer reactivity of twisted bilayer graphene when paired with an appropriate redox couple—a paired set of chemicals often used in energy storage to shuttle electrons between battery electrodes.

Adding an additional layer of graphene to make twisted trilayer graphene yielded a faster electron transfer compared to bilayer graphene, according to an electrochemical activity model in a recent study by University of Michigan researchers.

“We have discovered highly flexible and enhanced charge transfer reactivity in twisted trilayer graphene, which is not restricted to specific twist angles or redox couples,” said Venkat Viswanathan , an associate professor of aerospace engineering and corresponding author of the study published in the Journal of the American Chemical Society.

Stacking three layers of graphene introduced an additional twist angle, creating “incommensurate”, meaning non-repeating patterns, at small-angle twists—unlike bilayer graphene which forms repeating patterns. Essentially, when adding a third layer, the hexagonal lattices do not perfectly align.

electrochemistry experiments

Left: Periodic atomic structure of the magic angle in trilayer graphene. Right: Non-periodic atomic structure of the incommensurate angle in trilayer graphene. Image credit: Babar et al. 2024

[Left: Hexagonal repeating pattern of blue, orange, and yellow. Right: A non-repeating hexagonal pattern.]

At room temperature, these non-repeating patterns have a wider range of angles with high density of states away from the flat bands, increasing electrical conductivity comparable to those predicted at the magic angle.

“This discovery makes fabrication easier, avoiding the challenge of ensuring the precise twist angle that bilayer graphene requires,” said Mohammad Babar, a doctoral student of mechanical and aerospace engineering and first author of the study.

As a next step, the researchers plan to verify these findings in experiments and potentially discover even higher activity in multi-layer twisted 2D materials for a wide range of electrochemical processes such as redox reactions and electrocatalysis.

“Our work opens a new field of kinetics in 2D materials, capturing the electrochemical signatures of commensurate and incommensurate structures. We can now identify the optimal balance of charge transfer reactivity in trilayer graphene for a given redox couple,” said Babar.

This work was funded in part by the Simons Foundation (Award no. 896626) and computational resources were provided by the Extreme Science and Engineering Discovery Environment (Award No. TG-CTS180061).

Additional co-authors: Ziyan Zhu of the SLAC National Accelerator Laboratory, Rachel Kurchin of Carnegie Mellon University, Efthimios Kaxiras of Harvard University.

Full citation: “Twisto-Electrochemical Activity Volcanoes in Trilayer Graphene,” Mohammad Babar, Ziyan Zhu, Rachel Kurchin, Efthimios Kaxiras, and Venkatasubramanian Viswanathan, Journal of American Chemical Society (2024). DOI: 10.1021/jacs.4c03464

Left: Trilayer graphene twisted by θ12 and θ23, exchanging an electron from a redox couple, ruthenium hexamine. Center: Density of states (DoS) of trilayer graphene at the magic angle in red (1.1°/4.7°) and the incommensurate angle in blue (2.7°/4.7°). Right: Periodic atomic structure of the magic angle and non-periodic atomic structure of the incommensurate angle. Image credit: Babar et al. 2024

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Synthetic fuels and chemicals from CO₂: Ten experiments in parallel

by Anna Ettlin, Swiss Federal Laboratories for Materials Science and Technology

Synthetic fuels and chemicals from CO₂: Ten experiments in parallel

If you mix fossil fuel with a little oxygen and add a spark, three things are produced: water, climate-warming carbon dioxide, and lots of energy. This fundamental chemical reaction takes place in every combustion engine, whether it runs on gasoline, petrol, or kerosene. In theory, this reaction can be reversed: with the addition of (renewable) energy, previously released CO 2 can be converted back into a (synthetic) fuel.

This was the key idea behind the Joint Initiative SynFuels. Researchers at Empa and the Paul Scherrer Institute (PSI) spent three years working on ways to produce synthetic fuels—known as synfuels—economically and efficiently from CO 2 .

This reaction, however, comes with challenges: For one, CO 2 electrolysis does not just yield the fuel that was previously burned. Rather, more than 20 different products can be simultaneously formed, and they are difficult to separate from each other.

The composition of these products can be controlled in various ways, for example via the reaction conditions , the catalyst used, and the microstructure of the electrodes. The number of possible combinations is enormous and examining each one individually would take too long. How are scientists supposed to find the best one? Empa researchers have now accelerated this process by a factor of 10.

Accelerating research

As part of the SynFuels project, researchers led by Corsin Battaglia and Alessandro Senocrate from Empa's Materials for Energy Conversion laboratory have developed a system that can be used to investigate up to 10 different reaction conditions as well as catalyst and electrode materials simultaneously. The researchers have recently published the blueprint for the system and the accompanying software in the journal Nature Catalysis .

The system consists of 10 "reactors": small chambers with catalysts and electrodes in which the reaction takes place. Each reactor is connected to multiple gas and liquid in- and outlets and various instruments via hundreds of meters of tubing. Numerous parameters are recorded fully automatically, such as the pressure, the temperature, gas flows, and the liquid and gaseous reaction products—all with high temporal resolution.

"As far as we know, this is the first system of its kind for CO 2 electrolysis," says Empa postdoctoral researcher Alessandro Senocrate. "It yields a large number of high-quality datasets, which will help us make accelerated discoveries."

When the system was being developed, some of the necessary instruments were not even available on the market. In collaboration with the company Agilent Technologies, Empa researchers co-developed the world's first online liquid chromatography device, which identifies and quantifies the liquid reaction products in real time during CO 2 electrolysis.

Sharing research data

Conducting experiments 10 times faster also generates 10 times as much data. In order to analyze this data, the researchers have developed a software solution that they are making available to scientists at other institutions on an open-source basis. They also want to share the data itself with other researchers.

"Today, research data often disappears in a drawer as soon as the results are published," explains Corsin Battaglia, Head of Empa's Materials for Energy Conversion laboratory. A joint research project between Empa, PSI and ETH Zurich, which bears the name PREMISE, aims to prevent this. "We want to create standardized methods for storing and sharing data," says Battaglia. "Then other researchers can gain new insights from our data—and vice versa."

Open access to research data is also a priority in other research activities of the Materials for Energy Conversion laboratory. This includes the National Center of Competence in Research NCCR Catalysis, which focuses on sustainable chemistry.

The new parallel CO 2 electrolysis system is set to play an important role in the second phase of this large-scale national project, with both the data generated and the know-how made available to other Swiss research institutions. To this end, the Empa researchers will continue to refine both the hardware and the software in the future.

Journal information: Nature Catalysis

Provided by Swiss Federal Laboratories for Materials Science and Technology

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