how is experimental error

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How to Calculate Experimental Error in Chemistry

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• Ph.D., Biomedical Sciences, University of Tennessee at Knoxville
• B.A., Physics and Mathematics, Hastings College

Error is a measure of accuracy of the values in your experiment. It is important to be able to calculate experimental error, but there is more than one way to calculate and express it. Here are the most common ways to calculate experimental error:

Error Formula

In general, error is the difference between an accepted or theoretical value and an experimental value.

Error = Experimental Value - Known Value

Relative Error Formula

Relative Error = Error / Known Value

Percent Error Formula

% Error = Relative Error x 100%

Example Error Calculations

Let's say a researcher measures the mass of a sample to be 5.51 grams. The actual mass of the sample is known to be 5.80 grams. Calculate the error of the measurement.

Experimental Value = 5.51 grams Known Value = 5.80 grams

Error = Experimental Value - Known Value Error = 5.51 g - 5.80 grams Error = - 0.29 grams

Relative Error = Error / Known Value Relative Error = - 0.29 g / 5.80 grams Relative Error = - 0.050

% Error = Relative Error x 100% % Error = - 0.050 x 100% % Error = - 5.0%

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Systematic vs Random Error – Differences and Examples

Systematic and random error are an inevitable part of measurement. Error is not an accident or mistake. It naturally results from the instruments we use, the way we use them, and factors outside our control. Take a look at what systematic and random error are, get examples, and learn how to minimize their effects on measurements.

• Systematic error has the same value or proportion for every measurement, while random error fluctuates unpredictably.
• Systematic error primarily reduces measurement accuracy, while random error reduces measurement precision.
• It’s possible to reduce systematic error, but random error cannot be eliminated.

Systematic vs Random Error

Systematic error is consistent, reproducible error that is not determined by chance. Systematic error introduces inaccuracy into measurements, even though they may be precise. Averaging repeated measurements does not reduce systematic error, but calibrating instruments helps. Systematic error always occurs and has the same value when repeating measurements the same way.

As its name suggests, random error is inconsistent error caused by chance differences that occur when taking repeated measurements. Random error reduces measurement precision, but measurements cluster around the true value. Averaging measurements containing only random error gives an accurate, imprecise value. Random errors cannot be controlled and are not the same from one measurement to the next.

Systematic Error Examples and Causes

Systematic error is consistent or proportional to the measurement, so it primarily affects accuracy. Causes of systematic error include poor instrument calibration, environmental influence, and imperfect measurement technique.

Here are examples of systematic error:

• Reading a meniscus above or below eye level always gives an inaccurate reading. The reading is consistently high or low, depending on the viewing angle.
• A scale gives a mass measurement that is always “off” by a set amount. This is called an offset error . Taring or zeroing a scale counteracts this error.
• Metal rulers consistently give different measurements when they are cold compared to when they are hot due to thermal expansion. Reducing this error means using a ruler at the temperature at which it was calibrated.
• An improperly calibrated thermometer gives accurate readings within a normal temperature range. But, readings become less accurate at higher or lower temperatures.
• An old, stretched cloth measuring tape gives consistent, but different measurements than a new tape. Proportional errors of this type are called scale factor errors .
• Drift occurs when successive measurements become consistently higher or lower as time progresses. Electronic equipment is susceptible to drift. Devices that warm up tend to experience positive drift. In some cases, the solution is to wait until an instrument warms up before using it. In other cases, it’s important to calibrate equipment to account for drift.

How to Reduce Systematic Error

Once you recognize systematic error, it’s possible to reduce it. This involves calibrating equipment, warming up instruments because taking readings, comparing values against standards, and using experimental controls. You’ll get less systematic error if you have experience with a measuring instrument and know its limitations. Randomizing sampling methods also helps, particularly when drift is a concern.

Random Error Examples and Causes

Random error causes measurements to cluster around the true value, so it primarily affects precision. Causes of random error include instrument limitations, minor variations in measuring techniques, and environmental factors.

Here are examples of random error:

• Posture changes affect height measurements.
• Reaction speed affects timing measurements.
• Slight variations in viewing angle affect volume measurements.
• Wind velocity and direction measurements naturally vary according to the time at which they are taken. Averaging several measurements gives a more accurate value.
• Readings that fall between the marks on a device must be estimated. To some extent, its possible to minimize this error by choosing an appropriate instrument. For example, volume measurements are more precise using a graduated cylinder instead of a beaker.
• Mass measurements on an analytical balance vary with air currents and tiny mass changes in the sample.
• Weight measurements on a scale vary because it’s impossible to stand on the scale exactly the same way each time. Averaging multiple measurements minimizes the error.

How to Reduce Random Error

It’s not possible to eliminate random error, but there are ways to minimize its effect. Repeat measurements or increase sample size. Be sure to average data to offset the influence of chance.

Which Types of Error Is Worse?

Systematic errors are a bigger problem than random errors. This is because random errors affect precision, but it’s possible to average multiple measurements to get an accurate value. In contrast, systematic errors affect precision. Unless the error is recognized, measurements with systematic errors may be far from true values.

• Bland, J. Martin, and Douglas G. Altman (1996). “Statistics Notes: Measurement Error.”  BMJ  313.7059: 744.
• Cochran, W. G. (1968). “Errors of Measurement in Statistics”.  Technometrics . Taylor & Francis, Ltd. on behalf of American Statistical Association and American Society for Quality. 10: 637–666. doi: 10.2307/1267450
• Dodge, Y. (2003).  The Oxford Dictionary of Statistical Terms . OUP. ISBN 0-19-920613-9.
• Taylor, J. R. (1999).  An Introduction to Error Analysis: The Study of Uncertainties in Physical Measurements . University Science Books. ISBN 0-935702-75-X.

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• > A Practical Guide to Data Analysis for Physical Science Students
• > Experimental errors

Book contents

• Frontmatter
• Glossary and Conventions
• 1 Experimental errors
• 2 Least squares fitting
• Appendix 1 Useful formulae
• Appendix 2 Partial differentiation
• Appendix 3 The binomial distribution
• Appendix 4 The Poisson distribution
• Appendix 5 Student's t distribution
• Appendix 6 Statistical tables
• Appendix 7 Random numbers

1 - Experimental errors

Published online by Cambridge University Press:  05 June 2012

Why estimate errors?

When performing experiments at school, we usually considered that the job was over once we obtained a numerical value for the quantity we were trying to measure. At university, and even more so in everyday situations in the laboratory, we are concerned not only with the answer but also with its accuracy. This accuracy is expressed by quoting an experimental error on the quantity of interest. Thus a determination of the acceleration due to gravity in our laboratory might yield an answer

g = (9.70 ± 0.15) m/s 2 .

In Section 1.4, we will say more specifically what we mean by the error of ±0.15. At this stage it is sufficient to state that the more accurate the experiment the smaller the error; and that the numerical value of the error gives an indication of how far from the true answer this particular experiment may be.

The reason we are so insistent on every measurement including an error estimate is as follows. Scientists are rarely interested in measurement for its own sake, but more often will use it to test a theory, to compare with other experiments measuring the same quantity, to use this parameter to help predict the result of a different experiment, and so on. Then the numerical value of the error becomes crucial in the interpretation of the result.

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• Experimental errors
• Louis Lyons
• Book: A Practical Guide to Data Analysis for Physical Science Students
• Online publication: 05 June 2012
• Chapter DOI: https://doi.org/10.1017/CBO9781139170321.003

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Types of Error — Overview & Comparison - Expii

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Methodology

• Guide to Experimental Design | Overview, Steps, & Examples

Guide to Experimental Design | Overview, 5 steps & Examples

Published on December 3, 2019 by Rebecca Bevans . Revised on June 21, 2023.

Experiments are used to study causal relationships . You manipulate one or more independent variables and measure their effect on one or more dependent variables.

Experimental design create a set of procedures to systematically test a hypothesis . A good experimental design requires a strong understanding of the system you are studying.

There are five key steps in designing an experiment:

• Consider your variables and how they are related
• Write a specific, testable hypothesis
• Design experimental treatments to manipulate your independent variable
• Assign subjects to groups, either between-subjects or within-subjects
• Plan how you will measure your dependent variable

For valid conclusions, you also need to select a representative sample and control any  extraneous variables that might influence your results. If random assignment of participants to control and treatment groups is impossible, unethical, or highly difficult, consider an observational study instead. This minimizes several types of research bias, particularly sampling bias , survivorship bias , and attrition bias as time passes.

Table of contents

Step 1: define your variables, step 2: write your hypothesis, step 3: design your experimental treatments, step 4: assign your subjects to treatment groups, step 5: measure your dependent variable, other interesting articles, frequently asked questions about experiments.

You should begin with a specific research question . We will work with two research question examples, one from health sciences and one from ecology:

To translate your research question into an experimental hypothesis, you need to define the main variables and make predictions about how they are related.

Start by simply listing the independent and dependent variables .

Then you need to think about possible extraneous and confounding variables and consider how you might control  them in your experiment.

Finally, you can put these variables together into a diagram. Use arrows to show the possible relationships between variables and include signs to show the expected direction of the relationships.

Here we predict that increasing temperature will increase soil respiration and decrease soil moisture, while decreasing soil moisture will lead to decreased soil respiration.

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Professional editors proofread and edit your paper by focusing on:

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Now that you have a strong conceptual understanding of the system you are studying, you should be able to write a specific, testable hypothesis that addresses your research question.

The next steps will describe how to design a controlled experiment . In a controlled experiment, you must be able to:

• Systematically and precisely manipulate the independent variable(s).
• Precisely measure the dependent variable(s).
• Control any potential confounding variables.

If your study system doesn’t match these criteria, there are other types of research you can use to answer your research question.

How you manipulate the independent variable can affect the experiment’s external validity – that is, the extent to which the results can be generalized and applied to the broader world.

First, you may need to decide how widely to vary your independent variable.

• just slightly above the natural range for your study region.
• over a wider range of temperatures to mimic future warming.
• over an extreme range that is beyond any possible natural variation.

Second, you may need to choose how finely to vary your independent variable. Sometimes this choice is made for you by your experimental system, but often you will need to decide, and this will affect how much you can infer from your results.

• a categorical variable : either as binary (yes/no) or as levels of a factor (no phone use, low phone use, high phone use).
• a continuous variable (minutes of phone use measured every night).

How you apply your experimental treatments to your test subjects is crucial for obtaining valid and reliable results.

First, you need to consider the study size : how many individuals will be included in the experiment? In general, the more subjects you include, the greater your experiment’s statistical power , which determines how much confidence you can have in your results.

Then you need to randomly assign your subjects to treatment groups . Each group receives a different level of the treatment (e.g. no phone use, low phone use, high phone use).

You should also include a control group , which receives no treatment. The control group tells us what would have happened to your test subjects without any experimental intervention.

When assigning your subjects to groups, there are two main choices you need to make:

• A completely randomized design vs a randomized block design .
• A between-subjects design vs a within-subjects design .

Randomization

An experiment can be completely randomized or randomized within blocks (aka strata):

• In a completely randomized design , every subject is assigned to a treatment group at random.
• In a randomized block design (aka stratified random design), subjects are first grouped according to a characteristic they share, and then randomly assigned to treatments within those groups.

Sometimes randomization isn’t practical or ethical , so researchers create partially-random or even non-random designs. An experimental design where treatments aren’t randomly assigned is called a quasi-experimental design .

Between-subjects vs. within-subjects

In a between-subjects design (also known as an independent measures design or classic ANOVA design), individuals receive only one of the possible levels of an experimental treatment.

In medical or social research, you might also use matched pairs within your between-subjects design to make sure that each treatment group contains the same variety of test subjects in the same proportions.

In a within-subjects design (also known as a repeated measures design), every individual receives each of the experimental treatments consecutively, and their responses to each treatment are measured.

Within-subjects or repeated measures can also refer to an experimental design where an effect emerges over time, and individual responses are measured over time in order to measure this effect as it emerges.

Counterbalancing (randomizing or reversing the order of treatments among subjects) is often used in within-subjects designs to ensure that the order of treatment application doesn’t influence the results of the experiment.

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Finally, you need to decide how you’ll collect data on your dependent variable outcomes. You should aim for reliable and valid measurements that minimize research bias or error.

Some variables, like temperature, can be objectively measured with scientific instruments. Others may need to be operationalized to turn them into measurable observations.

• Ask participants to record what time they go to sleep and get up each day.
• Ask participants to wear a sleep tracker.

How precisely you measure your dependent variable also affects the kinds of statistical analysis you can use on your data.

Experiments are always context-dependent, and a good experimental design will take into account all of the unique considerations of your study system to produce information that is both valid and relevant to your research question.

If you want to know more about statistics , methodology , or research bias , make sure to check out some of our other articles with explanations and examples.

• Student’s  t -distribution
• Normal distribution
• Null and Alternative Hypotheses
• Chi square tests
• Confidence interval
• Cluster sampling
• Stratified sampling
• Data cleansing
• Reproducibility vs Replicability
• Peer review
• Likert scale

Research bias

• Implicit bias
• Framing effect
• Cognitive bias
• Placebo effect
• Hawthorne effect
• Hindsight bias
• Affect heuristic

Experimental design means planning a set of procedures to investigate a relationship between variables . To design a controlled experiment, you need:

• A testable hypothesis
• At least one independent variable that can be precisely manipulated
• At least one dependent variable that can be precisely measured

When designing the experiment, you decide:

• How you will manipulate the variable(s)
• How you will control for any potential confounding variables
• How many subjects or samples will be included in the study
• How subjects will be assigned to treatment levels

Experimental design is essential to the internal and external validity of your experiment.

The key difference between observational studies and experimental designs is that a well-done observational study does not influence the responses of participants, while experiments do have some sort of treatment condition applied to at least some participants by random assignment .

A confounding variable , also called a confounder or confounding factor, is a third variable in a study examining a potential cause-and-effect relationship.

A confounding variable is related to both the supposed cause and the supposed effect of the study. It can be difficult to separate the true effect of the independent variable from the effect of the confounding variable.

In your research design , it’s important to identify potential confounding variables and plan how you will reduce their impact.

In a between-subjects design , every participant experiences only one condition, and researchers assess group differences between participants in various conditions.

In a within-subjects design , each participant experiences all conditions, and researchers test the same participants repeatedly for differences between conditions.

The word “between” means that you’re comparing different conditions between groups, while the word “within” means you’re comparing different conditions within the same group.

An experimental group, also known as a treatment group, receives the treatment whose effect researchers wish to study, whereas a control group does not. They should be identical in all other ways.

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• Published: 11 November 2022

Error, reproducibility and uncertainty in experiments for electrochemical energy technologies

• Graham Smith   ORCID: orcid.org/0000-0003-0713-2893 1 &
• Edmund J. F. Dickinson   ORCID: orcid.org/0000-0003-2137-3327 1  

Nature Communications volume  13 , Article number:  6832 ( 2022 ) Cite this article

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• Electrocatalysis
• Electrochemistry
• Materials for energy and catalysis

The authors provide a metrology-led perspective on best practice for the electrochemical characterisation of materials for electrochemical energy technologies. Such electrochemical experiments are highly sensitive, and their results are, in practice, often of uncertain quality and challenging to reproduce quantitatively.

A critical aspect of research on electrochemical energy devices, such as batteries, fuel cells and electrolysers, is the evaluation of new materials, components, or processes in electrochemical cells, either ex situ, in situ or in operation. For such experiments, rigorous experimental control and standardised methods are required to achieve reproducibility, even on standard or idealised systems such as single crystal platinum 1 . Data reported for novel materials often exhibit high (or unstated) uncertainty and often prove challenging to reproduce quantitatively. This situation is exacerbated by a lack of formally standardised methods, and practitioners with less formal training in electrochemistry being unaware of best practices. This limits trust in published metrics, with discussions on novel electrochemical systems frequently focusing on a single series of experiments performed by one researcher in one laboratory, comparing the relative performance of the novel material against a claimed state-of-the-art.

Much has been written about the broader reproducibility/replication crisis 2 and those reading the electrochemical literature will be familiar with weakly underpinned claims of “outstanding” performance, while being aware that comparisons may be invalidated by measurement errors introduced by experimental procedures which violate best practice; such issues frequently mar otherwise exciting science in this area. The degree of concern over the quality of reported results is evidenced by the recent decision of several journals to publish explicit experimental best practices 3 , 4 , 5 , reporting guidelines or checklists 6 , 7 , 8 , 9 , 10 and commentary 11 , 12 , 13 aiming to improve the situation, including for parallel theoretical work 14 .

We write as two electrochemists who, working in a national metrology institute, have enjoyed recent exposure to metrology: the science of measurement. Metrology provides the vocabulary 15 and mathematical tools 16 to express confidence in measurements and the comparisons made between them. Metrological systems and frameworks for quantification underpin consistency and assurance in all measurement fields and formal metrology is an everyday consideration for practical and academic work in fields where accurate measurements are crucial; we have found it a useful framework within which to evaluate our own electrochemical work. Here, rather than pen another best practice guide, we aim, with focus on three-electrode electrochemical measurements for energy material characterisation, to summarise some advice that we hope helps those performing electrochemical experiments to:

avoid mistakes and minimise error

report in a manner that facilitates reproducibility

consider and quantify uncertainty

Minimising mistakes and error

Metrology dispenses with nebulous concepts such as performance and instead requires scientists to define a specific measurand (“the quantity intended to be measured”) along with a measurement model ( ”the mathematical relation among all quantities known to be involved in a measurement”), which converts the experimental indicators into the measurand 15 . Error is the difference between the reported value of this measurand and its unknowable true value. (Note this is not the formal definition, and the formal concepts of error and true value are not fully compatible with measurement concepts discussed in this article, but we retain it here—as is common in metrology tuition delivered by national metrology institutes—for pedagogical purposes 15 ).

Mistakes (or gross errors) are those things which prevent measurements from working as intended. In electrochemistry the primary experimental indicator is often current or voltage, while the measurand might be something simple, like device voltage for a given current density, or more complex, like a catalyst’s turnover frequency. Both of these are examples of ‘method-defined measurands’, where the results need to be defined in reference to the method of measurement 17 , 18 (for example, to take account of operating conditions). Robust experimental design and execution are vital to understand, quantify and minimise sources of error, and to prevent mistakes.

Contemporary electrochemical instrumentation can routinely offer a current resolution and accuracy on the order of femtoamps; however, one electron looks much like another to a potentiostat. Consequently, the practical limit on measurements of current is the scientist’s ability to unambiguously determine what causes the observed current. Crucially, they must exclude interfering processes such as modified/poisoned catalyst sites or competing reactions due to impurities.

As electrolytes are conventionally in enormous excess compared to the active heterogeneous interface, electrolyte purity requirements are very high. Note, for example, that a perfectly smooth 1 cm 2 polycrystalline platinum electrode has on the order of 2 nmol of atoms exposed to the electrolyte, so that irreversibly adsorbing impurities present at the part per billion level (nmol mol −1 ) in the electrolyte may substantially alter the surface of the electrode. Sources of impurities at such low concentration are innumerable and must be carefully considered for each experiment; impurity origins for kinetic studies in aqueous solution have been considered broadly in the historical literature, alongside a review of standard mitigation methods 19 . Most commercial electrolytes contain impurities and the specific ‘grade’ chosen may have a large effect; for example, one study showed a three-fold decrease in the specific activity of oxygen reduction catalysts when preparing electrolytes with American Chemical Society (ACS) grade acid rather than a higher purity grade 20 . Likewise, even 99.999% pure hydrogen gas, frequently used for sparging, may contain more than the 0.2 μmol mol −1 of carbon monoxide permitted for fuel cell use 21 .

The most insidious impurities are those generated in situ. The use of reference electrodes with chloride-containing filling solutions should be avoided where chloride may poison catalysts 22 or accelerate dissolution. Similarly, reactions at the counter electrode, including dissolution of the electrode itself, may result in impurities. This is sometimes overlooked when platinum counter electrodes are used to assess ‘platinum-free’ electrocatalysts, accidentally resulting in performance-enhancing contamination 23 , 24 ; a critical discussion on this topic has recently been published 25 . Other trace impurity sources include plasticisers present in cells and gaskets, or silicates from the inappropriate use of glass when working with alkaline electrolytes 26 . To mitigate sensitivity to impurities from the environment, cleaning protocols for cells and components must be robust 27 . The use of piranha solution or similarly oxidising solution followed by boiling in Type 1 water is typical when performing aqueous electrochemistry 20 . Cleaned glassware and electrodes are also routinely stored underwater to prevent recontamination from airborne impurities.

The behaviour of electronic hardware used for electrochemical experiments should be understood and considered carefully in interpreting data 28 , recognising that the built-in complexity of commercially available digital potentiostats (otherwise advantageous!) is capable of introducing measurement artefacts or ambiguity 29 , 30 . While contemporary electrochemical instrumentation may have a voltage resolution of ~1 μV, its voltage measurement uncertainty is limited by other factors, and is typically on the order of 1 mV. As passing current through an electrode changes its potential, a dedicated reference electrode is often incorporated into both ex situ and, increasingly, in situ experiments to provide a stable well defined reference. Reference electrodes are typically selected from a range of well-known standardised electrode–electrolyte interfaces at which a characteristic and kinetically rapid reversible faradaic process occurs. The choice of reference electrode should be made carefully in consideration of chemical compatibility with the measurement environment 31 , 32 , 33 , 34 . In combination with an electronic blocking resistance, the potential of the electrode should be stable and reproducible. Unfortunately, deviation from the ideal behaviour frequently occurs. While this can often be overlooked when comparing results from identical cells, more attention is required when reporting values for comparison.

In all cases where conversion between different electrolyte–reference electrode systems is required, junction potentials should be considered. These arise whenever there are different chemical conditions in the electrolyte at the working electrode and reference electrode interfaces. Outside highly dilute solutions, or where there are large activity differences for a reactant/product of the electrode reaction (e.g. pH for hydrogen reactions), liquid junction potentials for conventional aqueous ions have been estimated in the range <50 mV 33 . Such a deviation may nonetheless be significant when onset potentials or activities at specific potentials are being reported. The measured potential difference between the working and reference electrode also depends strongly on the geometry of the cell, so cell design is critical. Fig.  1 shows the influence of cell design on potential profiles. Ideally the reference electrode should therefore be placed close to the working electrode (noting that macroscopic electrodes may have inhomogeneous potentials). To minimise shielding of the electric field between counter and working electrode and interruption of mass transport processes, a thin Luggin-Haber capillary is often used and a small separation maintained. Understanding of shielding and edge effects is vital when reference electrodes are introduced in situ. This is especially applicable for analysis of energy devices for which constraints on cell design, due to the need to minimise electrolyte resistance and seal the cell, preclude optimal reference electrode positioning 32 , 35 , 36 .

a Illustration (simulated data) of primary (resistive) current and potential distribution in a typical three-electrode cell. The main compartment is cylindrical (4 cm diameter, 1 cm height), filled with electrolyte with conductivity 1.28 S m −1 (0.1 M KCl(aq)). The working electrode (WE) is a 2 mm diameter disc drawing 1 mA (≈ 32 mA cm −2 ) from a faradaic process with infinitely fast kinetics and redox potential 0.2 V vs the reference electrode (RE). The counter electrode (CE) is connected to the main compartment by a porous frit; the RE is connected by a Luggin capillary (green cylinders) whose tip position is offset from the WE by a variable distance. Red lines indicate prevailing current paths; coloured surfaces indicate isopotential contours normal to the current density. b Plot of indicated WE vs RE potential (simulated data). As the Luggin tip is moved away from the WE surface, ohmic losses due to the WE-CE current distribution lead to variation in the indicated WE-RE potential. Appreciable error may arise on an offset length scale comparable to the WE radius.

Quantitative statements about fundamental electrochemical processes based on measured values of current and voltage inevitably rely on models of the system. Such models have assumptions that may be routinely overlooked when following experimental and analysis methods, and that may restrict their application to real-world systems. It is quite possible to make highly precise but meaningless measurements! An often-assumed condition for electrocatalyst analysis is the absence of mass transport limitation. For some reactions, such as the acidic hydrogen oxidation and hydrogen evolution reactions, this state is arguably so challenging to reach at representative conditions that it is impossible to measure true catalyst activity 11 . For example, ex situ thin-film rotating disk electrode measurements routinely fail to predict correct trends in catalyst performance in morphologically complex catalyst layers  as relevant operating conditions (e.g. meaningful current densities) are theoretically inaccessible. This topic has been extensively discussed with some authors directly criticising this technique and exploring alternatives 37 , 38 , and others defending the technique’s applicability for ranking catalysts if scrupulous attention is paid to experimental details 39 ; yet, many reports continue to use this measurement technique blindly with no regard for its applicability. We therefore strongly urge those planning measurements to consider whether their chosen technique is capable of providing sufficient evidence to disprove their hypothesis, even if it has been widely used for similar experiments.

The correct choice of technique should be dependent upon the measurand being probed rather than simply following previous reports. The case of iR correction, where a measurement of the uncompensated resistance is used to correct the applied voltage, is a good example. When the measurand is a material property, such as intrinsic catalyst activity, the uncompensated resistance is a source of error introduced by the experimental method and it should carefully be corrected out (Fig.  1 ). In the case that the uncompensated resistance is intrinsic to the measurand—for instance the operating voltage of an electrolyser cell—iR compensation is inappropriate and only serves to obfuscate. Another example is the choice of ex situ (outside the operating environment), in situ (in the operating environment), and operando (during operation) measurements. While in situ or operando testing allows characterisation under conditions that are more representative of real-world use, it may also yield measurements with increased uncertainty due to the decreased possibility for fine experimental control. Depending on the intended use of the measurement, an informed compromise must be sought between how relevant and how uncertain the resulting measurement will be.

Maximising reproducibility

Most electrochemists assess the repeatability of measurements, performing the same measurement themselves several times. Repeats, where all steps (including sample preparation, where relevant) of a measurement are carried out multiple times, are absolutely crucial for highlighting one-off mistakes (Fig.  2 ). Reproducibility, however, is assessed when comparing results reported by different laboratories. Many readers will be familiar with the variability in key properties reported for various systems e.g. variability in the reported electrochemically active surface area (ECSA) of commercial catalysts, which might reasonably be expected to be constant, suggesting that, in practice, the reproducibility of results cannot be taken for granted. As electrochemistry deals mostly with method-defined measurands, the measurement procedure must be standardised for results to be comparable. Variation in results therefore strongly suggests that measurements are not being performed consistently and that the information typically supplied when publishing experimental methods is insufficient to facilitate reproducibility of electrochemical measurements. Quantitative electrochemical measurements require control over a large range of parameters, many of which are easily overlooked or specified imprecisely when reporting data. An understanding of the crucial parameters and methods for their control is often institutional knowledge, held by expert electrochemists, but infrequently formalised and communicated e.g. through publication of widely adopted standards. This creates challenges to both reproducibility and the corresponding assessment of experimental quality by reviewers. The reporting standards established by various publishers (see Introduction) offer a practical response, but it is still unclear whether these will contain sufficiently granular detail to improve the situation.

The measurements from laboratory 1 show a high degree of repeatability, while the measurements from laboratory 2 do not. Apparently, a mistake has been made in repeat 1, which will need to be excluded from any analysis and any uncertainty analysis, and/or suggests further repeat measurements should be conducted. The error bars are based on an uncertainty with coverage factor ~95% (see below) so the results from the two laboratories are different, i.e. show poor reproducibility. This may indicate differing experimental practice or that some as yet unidentified parameter is influencing the results.

Besides information typically supplied in the description of experimental methods for publication, which, at a minimum, must detail the materials, equipment and measurement methods used to generate the results, we suggest that a much more comprehensive description is often required, especially where measurements have historically poor reproducibility or the presented results differ from earlier reports. Such an expanded ‘supplementary experimental’ section would additionally include any details that could impact the results: for example, material pre-treatment, detailed electrode preparation steps, cleaning procedures, expected electrolyte and gas impurities, electrode preconditioning processes, cell geometry including electrode positions, detail of junctions between electrodes, and any other fine experimental details which might be institutional knowledge but unknown to the (now wide) readership of the electrochemical literature. In all cases any corrections and calculations used should be specified precisely and clearly justified; these may include determinations of properties of the studied system, such as ECSA, or of the environment, such as air pressure. We highlight that knowledge of the ECSA is crucial for conventional reporting of intrinsic electrocatalyst activity, but is often very challenging to measure in a reproducible manner 40 , 41 .

To aid reproducibility we recommend regularly calibrating experimental equipment and doing so in a way that is traceable to primary standards realising the International System of Units (SI) base units. The SI system ensures that measurement units (such as the volt) are uniform globally and invariant over time. Calibration applies to direct experimental indicators, e.g. loads and potentiostats, but equally to supporting tools such as temperature probes, balances, and flow meters. Calibration of reference electrodes is often overlooked even though variations from ideal behaviour can be significant 42 and, as discussed above, are often the limit of accuracy on potential measurement. Sometimes reports will specify internal calibration against a known reaction (such as the onset of the hydrogen evolution reaction), but rarely detail regular comparisons to a local master electrode artefact such as a reference hydrogen electrode or explain how that artefact is traceable, e.g. through control of the filling solution concentration and measurement conditions. If reference is made to a standardised material (e.g. commercial Pt/C) the specified material should be both widely available and the results obtained should be consistent with prior reports.

Beyond calibration and reporting, the best test of reproducibility is to perform intercomparisons between laboratories, either by comparing results to identical experiments reported in the literature or, more robustly, through participation in planned intercomparisons (for example ‘round-robin’ exercises); we highlight a recent study applied to solid electrolyte characterisation as a topical example 43 . Intercomparisons are excellent at establishing the key features of an experimental method and the comparability of results obtained from different methods; moreover they provide a consensus against which other laboratories may compare themselves. However, performing repeat measurements for assessing repeatability and reproducibility cannot estimate uncertainty comprehensively, as it excludes systematic sources of uncertainty.

Assessing measurement uncertainty

Formal uncertainty evaluation is an alien concept to most electrochemists; even the best papers (as well as our own!) typically report only the standard deviation between a few repeats. Metrological best practice dictates that reported values are stated as the combination of a best estimate of the measurand, and an interval, and a coverage factor ( k ) which gives the probability of the true value being within that interval. For example, “the turnover frequency of the electrocatalyst is 1.0 ± 0.2 s −1 ( k  = 2)” 16 means that the scientist (having assumed normally distributed error) is 95% confident that the turnover frequency lies in the range 0.8–1.2 s −1 . Reporting results in such a way makes it immediately clear whether the measurements reliably support the stated conclusions, and enables meaningful comparisons between independent results even if their uncertainties differ (Fig.  3 ). It also encourages honesty and self-reflection about the shortcomings of results, encouraging the development of improved experimental techniques.

a Complete reporting of a measurement includes the best estimate of the measurand and an uncertainty and the probability the true value falls within the uncertainty reported. Here, the percentages indicate that a normal distribution has been assumed. b Horizontal bars indicate 95% confidence intervals from uncertainty analysis. The confidence intervals of measurements 1 and 2 overlap when using k  = 2, so it is not possible to say with 95% confidence that the result of the measurement 2 is higher than measurement 1, but it is possible to say this with 68% confidence, i.e. k  = 1. Measurement 3 has a lower uncertainty, so it is possible to say with 95% confidence that the value is higher than measurement 2.

Constructing such a statement and performing the underlying calculations often appears daunting, not least as there are very few examples for electrochemical systems, with pH measurements being one example to have been treated thoroughly 44 . However, a standard process for uncertainty analysis exists, as briefly outlined graphically in Fig.  4 . We refer the interested reader to both accessible introductory texts 45 and detailed step-by-step guides 16 , 46 . The first steps in the process are to state precisely what is being measured—the measurand—and identify likely sources of uncertainty. Even this qualitative effort is often revealing. Precision in the definition of the measurand (and how it is determined from experimental indicators) clarifies the selection of measurement technique and helps to assess its appropriateness; for example, where the measurand relates only to an instantaneous property of a specific physical object, e.g. the current density of a specific fuel cell at 0.65 V following a standardised protocol, we ignore all variability in construction, device history etc. and no error is introduced by the sample. Whereas, when the measurand is a material property, such as turnover frequency of a catalyst material with a defined chemistry and preparation method, variability related to the material itself and sample preparation will often introduce substantial uncertainty in the final result. In electrochemical measurements, errors may arise from a range of sources including the measurement equipment, fluctuations in operating conditions, or variability in materials and samples. Identifying these sources leads to the design of better-quality experiments. In essence, the subsequent steps in the calculation of uncertainty quantify the uncertainty introduced by each source of error and, by using a measurement model or a sensitivity analysis (i.e. an assessment of how the results are sensitive to variability in input parameters), propagate these to arrive at a final uncertainty on the reported result.

Possible sources of uncertainty are identified, and their standard uncertainty or probability distribution is determined by statistical analysis of repeat measurements (Type A uncertainties) or other evidence (Type B uncertainties). If required, uncertainties are then converted into the same unit as the measurand and adjusted for sensitivity, using a measurement model. Uncertainties are then combined either analytically using a standard approach or numerically to generate an overall estimate of uncertainty for the measurand (as indicated in Fig.  3a ).

Generally, given the historically poor understanding of uncertainty in electrochemistry, we promote increased awareness of uncertainty reporting standards and a focus on reporting measurement uncertainty with a level of detail that is appropriate to the claim made, or the scientific utilisation of the data. For example, where the primary conclusion of a paper relies on demonstrating that a material has the ‘highest ever X’ or ‘X is bigger than Y’ it is reasonable for reviewers to ask authors to quantify how confident they are in their measurement and statement. Additionally, where uncertainties are reported, even with error bars in numerical or graphical data, the method by which the uncertainty was determined should be stated, even if the method is consciously simple (e.g. “error bars indicate the sample standard deviation of n  = 3 measurements carried out on independent electrodes”). Unfortunately, we are aware of only sporadic and incomplete efforts to create formal uncertainty budgets for electrochemical measurements of energy technologies or materials, though work is underway in our group to construct these for some exemplar systems.

Electrochemistry has undoubtedly thrived without significant interaction with formal metrology; we do not urge an abrupt revolution whereby rigorous measurements become devalued if they lack additional arcane formality. Rather, we recommend using the well-honed principles of metrology to illuminate best practice and increase transparency about the strengths and shortcomings of reported experiments. From rethinking experimental design, to participating in laboratory intercomparisons and estimating the uncertainty on key results, the application of metrological principles to electrochemistry will result in more robust science.

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Acknowledgements

This work was supported by the National Measurement System of the UK Department of Business, Energy & Industrial Strategy. Andy Wain, Richard Brown and Gareth Hinds (National Physical Laboratory, Teddington, UK) provided insightful comments on the text.

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Smith, G., Dickinson, E.J.F. Error, reproducibility and uncertainty in experiments for electrochemical energy technologies. Nat Commun 13 , 6832 (2022). https://doi.org/10.1038/s41467-022-34594-x

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