ExperimentPrepareReferenceElectrode

ExperimentPrepareReferenceElectrode[ReferenceElectrodeModel]⟹Protocol

generates a Protocol for the preparation of a reference electrode of the given ReferenceElectrodeModel according to the model information.

ExperimentPrepareReferenceElectrode[SourceReferenceElectrode, TargetReferenceElectrodeModel]⟹Protocol

generates a Protocol to fill or refresh the reference solution of SourceReferenceElectrode and reset its Model to TargetReferenceElectrodeModel. If the provided SourceReferenceElectrode is a Model, an Object of this Model is selected first and prepared into a reference electrode of the TargetReferenceElectrodeModel.

ExperimentPrepareReferenceElectrode generates ReferenceElectrode Object(s) of provided Model[Item, Electrode, ReferenceElectrode]. The input ReferenceElectrode can be an unprepared blank ReferenceElectrode (without any reference solution filled-in) or a previously prepared ReferenceElectrode (with reference solution filled-in). To prepare the new ReferenceElectrode, the electrode's metal part and the inside of the electrode's glass tube are primed with the ReferenceSolution. The outside of the glass tube is washed with water and methanol. If the glass tube is filled with a previous reference solution, the glass tube will be emptied before the priming step. Once the ReferenceElectrode and the glass tube are flushed, the glass tube is filled with the ReferenceSolution, and the electrode is assembled to finish the preparation. The newly prepared ReferenceElectrode(s) can be used in electrochemical experiments, including Cyclic Voltammetry measurements.

Experimental Principles

Figure 1.1: Procedural overview of a reference electrode preparation experiment. For an unprepared blank reference electrode: Step 1: Disassemble input reference electrode. Step 2: The electrode metal part and the inside of the glass tube is flushed (primed) with the ReferenceSolution. The outside of the glass tube is washed with water and methanol. Step 3: The glass tube is filled with ReferenceSolution and assembled with the electrode metal part to finalize the preparation experiment. For a previous prepared reference electrode: Step 1: Disassemble input reference electrode(s). Step 2: The previous reference solution is aspirated out from the glass tube. Step 3: The electrode metal part and the inside of the glass tube is flushed (primed) with the ReferenceSolution. The outside of the glass tube is washed with water and methanol. Step 4: The glass tube is filled with ReferenceSolution and assembled with the electrode metal part to finalize the preparation experiment.

Instrumentation

IKA ElectraSyn 2.0

Figure 2.1.1: The IKA ElectraSyn 2.0 instrument has a cyclic voltammetry (CV) assembly, a potentiostat, and a data acquisition system. The CV assembly holds the sample solution and three electrodes: working electrode (WE), counter electrode (CE), and reference electrode (RE). The reduction / oxidation of the interested analyte happens at WE, and the corresponding counter reactions of another molecule species happens at CE, which completes the electrical circuit (but not of experimental interest). The potential of RE stays constant during the course of CV measurement. The sample solution contains three main parts: solvent, electrolyte, and sample analyte. The choice of the solvent should avoid reactions with electrolyte, analyte and three electrodes within the potential window (the potential range CV experiment carries out in). The solvent should also be able to dissolve a high concentration (0.05–0.5 M) of electrolyte, which is added to decrease the resistance of the sample solution while not interfering the analyte reactions. The concentration of the analyte should be kept in the range of 1–10 mM. Depending on the RE type, an internal standard chemical can also be added into the sample solution. During the course of CV experiment, the potentiostat uses a dc power source to produce a potential which can be maintained and accurately determined, while allowing small currents to be drawn into the system without changing the voltage. The potentiostat generates a cyclically and linear sweeping potential (-2.5–2.5 V, limited by the platinum coated CE) between the WE and CE. The potential between the WE and RE is measured as the output potential signal. The current that flows between WE and CE is measured to generate the output current signal. The data acquisition system collects the output current and potential signals to generate the final voltammogram.

Experiment Options

Electrode Polishing

PolishReferenceElectrode

Indicates if in the presence of rust, the non-working part (the metal part that does not directly contact experiment solution) of reference electrode is polished with a piece of 1200 grit sandpaper. The working part (the metal part that directly contacts experiment solution) will not be polished, and if rust is present on the working part, the electrode's RustyLog will be updated.

Default Value: True

Pattern Description: True or False.

Programmatic Pattern: BooleanP

Index Matches to: experiment samples

Electrode Cleaning

PrimaryWashingSolution

The solution used to wash the electrode metal wiring or plate and the electrode glass tube, after the previous reference solution (if any) is emptied and the optional polishing step is completed. This washing step helps to remove any remaining liquid or solid on the electrode metal wire or plate. A washing cycle includes rinsing the full surface areas of the electrode metal wiring or plate and the electrode glass tube (both inside and outside), with approximately 5 mL of solution.

Default Value: Automatic

Default Calculation: Automatically set to Model[Sample, "Milli-Q water"] if the RecommendedSolventType of the reference electrode model being prepared is Aqueous. If the RecommendedSolventType is Organic, it is automatically set to Model[Sample, "Acetonitrile, Electronic Grade"].

Pattern Description: An object of type or subtype Model[Sample] or Object[Sample] or a prepared sample or Null.

Programmatic Pattern: ((ObjectP[{Model[Sample], Object[Sample]}] | _String) | Automatic) | Null

Index Matches to: experiment samples

NumberOfPrimaryWashings

Indicates the number of washing cycles performed with PrimaryWashingSolution.

Default Value: Automatic

Default Calculation: Automatically set to 2 if PrimaryWashingSolution is not Null. Automatically set to Null if PrimaryWashingSolution is set to Null.

Pattern Description: Greater than or equal to 1 and less than or equal to 10 in increments of 1 or Null.

Programmatic Pattern: (RangeP[1, 10, 1] | Automatic) | Null

Index Matches to: experiment samples

SecondaryWashingSolution

The second solution used to wash the electrode metal wiring or plate and the electrode glass tube, after the primary washing step. This washing step helps to further remove any remaining liquid or solid on the electrode metal wire or plate. A washing cycle includes rinsing the full surface areas of the electrode metal wiring or plate and the electrode glass tube (both inside and outside), with approximately 5 mL of solution.

Default Value: Null

Pattern Description: An object of type or subtype Model[Sample] or Object[Sample] or a prepared sample or Null.

Programmatic Pattern: (ObjectP[{Model[Sample], Object[Sample]}] | _String) | Null

Index Matches to: experiment samples

NumberOfSecondaryWashings

Indicates the number of washing cycles performed with SecondaryWashingSolution.

Default Value: Automatic

Default Calculation: Automatically set to 2 if SecondaryWashingSolution is not Null. Automatically set to Null if SecondaryWashingSolution is set to Null.

Pattern Description: Greater than or equal to 1 and less than or equal to 10 in increments of 1 or Null.

Programmatic Pattern: (RangeP[1, 10, 1] | Automatic) | Null

Index Matches to: experiment samples

Reference Electrode Preparation

NumberOfPrimings

Indicates the number of priming cycles performed with ReferenceSolution defined in the reference electrode model being prepared. A priming cycle includes rinsing the full surface areas of the electrode metal wiring or plate and the electrode glass tube (only inside).

Default Value: 2

Pattern Description: Greater than or equal to 1 and less than or equal to 10 in increments of 1.

Programmatic Pattern: RangeP[1, 10, 1]

Index Matches to: experiment samples

PrimingVolume

Indicates the volume of the ReferenceSolution used to prime the reference electrode metal wire or plate and the inside of the glass tube in each priming cycle.

Default Value: Automatic

Default Calculation: Automatically set to the greater of 2 Milliliter or 2 times of the SolutionVolume defined in the reference electrode model being prepared.

Pattern Description: Greater than or equal to 0 milliliters and less than or equal to 20 milliliters.

Programmatic Pattern: RangeP[0*Milliliter, 20*Milliliter] | Automatic

Index Matches to: experiment samples

PrimingSoakTime

Indicates the minimum duration of the reference electrode metal wire or plate will be soaked in the ReferenceSolution within the glass tube after the last priming cycle.

Default Value: 5 minutes

Pattern Description: Greater than or equal to 1 minute and less than or equal to 15 minutes.

Programmatic Pattern: RangeP[1*Minute, 15*Minute]

Index Matches to: experiment samples

ReferenceSolutionVolume

Indicates the volume of the ReferenceSolution the electrode's glass tube is filled with. The ReferenceSolutionVolume should be within the range of 95% and 105% of the SolutionVolume defined by the reference electrode model being prepared.

Default Value: Automatic

Default Calculation: Automatically set to the SolutionVolume defined in the reference electrode model being prepared.

Pattern Description: Greater than 0 milliliters.

Programmatic Pattern: GreaterP[0*Milliliter] | Automatic

Index Matches to: experiment samples

Post Experiment

SamplesOutStorageCondition

The non-default conditions under which any new samples generated by this experiment should be stored after the protocol is completed. If left unset, the new samples will be stored according to their Models' DefaultStorageCondition.

Default Value: Null

Pattern Description: {AmbientStorage, Refrigerator, Freezer, DeepFreezer, CryogenicStorage, YeastIncubation, BacteriaIncubation, MammalianIncubation, TissueCultureCellsIncubation, MicrobialCellsIncubation, MicrobialCellsShakingIncubation, YeastCellsIncubation, YeastCellsShakingIncubation, ViralIncubation, AcceleratedTesting, IntermediateTesting, LongTermTesting, UVVisLightTesting} or Disposal or Null.

Programmatic Pattern: (Alternatives[SampleStorageTypeP | Disposal]) | Null

Index Matches to: experiment samples

Protocol

NumberOfReplicates

Number of times each of the input reference electrode model should be prepared using identical experimental parameters.

Default Value: Null

Pattern Description: Greater than or equal to 2 and less than or equal to 5 in increments of 1 or Null.

Programmatic Pattern: RangeP[2, 5, 1] | Null

Protocol Options

Organizational Information

Template

A template protocol whose methodology should be reproduced in running this experiment. Option values will be inherited from the template protocol, but can be individually overridden by directly specifying values for those options to this Experiment function.

Default Value: Null

Pattern Description: An object of type or subtype Object[Protocol] or an object of type or subtype of Object[Protocol] with UnresolvedOptions, ResolvedOptions specified or Null.

Programmatic Pattern: (ObjectP[Object[Protocol]] | FieldReferenceP[Object[Protocol], {UnresolvedOptions, ResolvedOptions}]) | Null

Name

A object name which should be used to refer to the output object in lieu of an automatically generated ID number.

Default Value: Null

Pattern Description: A string or Null.

Programmatic Pattern: _String | Null

Post Experiment

MeasureWeight

Indicates if any solid samples that are modified in the course of the experiment should have their weights measured and updated after running the experiment. Please note that public samples are weighed regardless of the value of this option.

Default Value: Automatic

Pattern Description: True or False or Null.

Programmatic Pattern: (BooleanP | Automatic) | Null

MeasureVolume

Indicates if any liquid samples that are modified in the course of the experiment should have their volumes measured and updated after running the experiment. Please note that public samples are volume measured regardless of the value of this option.

Default Value: Automatic

Pattern Description: True or False or Null.

Programmatic Pattern: (BooleanP | Automatic) | Null

ImageSample

Indicates if any samples that are modified in the course of the experiment should be freshly imaged after running the experiment. Please note that public samples are imaged regardless of the value of this option.

Default Value: Automatic

Pattern Description: True or False or Null.

Programmatic Pattern: (BooleanP | Automatic) | Null

Example Calls

Prepare Reference Electrodes of Given Models

Prepare a reference electrode of a given model:

Prepare several reference electrode of multiple given models:

Prepare Reference Electrodes Using Source Electrodes

Prepare a blank reference electrode into a given model:

Prepare several blank reference electrodes into several given models:

Pair the source reference electrodes with the corresponding target models:

Refresh a reference electrode with the reference solution defined in its corresponding reference electrode model:

Warnings and Errors

Messages (27)

Deprecated target reference electrode model (1)

If there are deprecated models in the input target reference electrode model(s), an error will be thrown:

Discarded input source reference electrodes (1)

If there are discarded electrodes in the input source reference electrode(s), an error will be thrown:

Duplicated input source reference electrodes (1)

If there are duplicated electrodes in the input source reference electrode list, an error will be thrown:

Mismatching Blank models (1)

If the target reference electrode's Blank model is different from the source reference electrode Blank model (when the source reference electrode itself is a Blank model) or the Blank model defined in source reference electrode, an error will be thrown:

Mismatching Lengths of source electrodes and target reference electrode models (1)

If the input source reference electrode list and the target reference electrode model list do have have the same length, an error will be thrown:

Missing PrimaryWashingSolution (1)

If the PrimaryWashingSolution is set to Null and SecondaryWashingSolution is set to a washing solution, an error will be thrown:

No reference electrode in the provided container (1)

If the a container without any reference electrode stored in it is used as the input, an error will be thrown:

Null PrimaryWashingSolution (1)

If the PrimaryWashingSolution is set to Null, a warning will be thrown:

Options with too high precisions (1)

If an option is given with higher precision than the instrument can achieve, the value is rounded to the instrument precision and a warning is displayed:

ReferenceCouplingSample Switching (1)

If the source reference electrode is not a Blank electrode or electrode model, and the target reference electrode model is of another ReferenceElectrodeType different from the source reference electrode, a warning will be thrown:

ReferenceElectrodeType Switching (1)

Same washing solutions (1)

If the PrimaryWashingSolution and SecondaryWashingSolution are set to the same washing solution, an error will be thrown:

Source reference electrode working part rust (1)

If the source reference electrode has rust observed on its working part (the part that directly contacts the experiment solution), a warning will be thrown:

Target reference electrode is a Blank model (1)

If input target reference electrode model is a Blank model (with its Blank field set to Null and does not have a reference solution defined), an error will be thrown:

Too many reference electrodes to be prepared (1)

If there are more than 10 target reference electrodes to be prepared, an error will be thrown:

Unpreparable target reference electrode model (1)

If there are unpreparable models in the input target reference electrode model(s), an error will be thrown:

NumberOfPrimaryWashings (2)

If the NumberOfPrimaryWashings is set to an integer when the PrimaryWashingSolution is set to Null, an error will be thrown:

If the NumberOfPrimaryWashings is set to Null when the PrimaryWashingSolution is set to a washing solution, an error will be thrown:

NumberOfReplicates (1)

If the NumberOfReplicates options is specified to an integer when there is at least one input source reference electrode Object, an error will be thrown:

NumberOfSecondaryWashings (2)

If the NumberOfSecondaryWashings is set to an integer when the SecondaryWashingSolution is set to Null, an error will be thrown:

If the NumberOfSecondaryWashings is set to Null when the SecondaryWashingSolution is set to a washing solution, an error will be thrown:

PolishReferenceElectrode (1)

If the input reference electrode has rust found on its non-working part (the part does not directly contact the experiment solution) and the PolishReferenceElectrode options is set to False, an error will be thrown:

PrimingVolume (1)

If the specified PrimingVolume is less than 1.5 Milliliter, an error will be thrown:

ReferenceSolutionVolume (2)

If the specified ReferenceSolutionVolume is greater than 105% of the SolutionVolume defined in the target reference electrode model, an error will be thrown:

If the specified ReferenceSolutionVolume is less than 95% of the SolutionVolume defined in the target reference electrode model, an error will be thrown:

SamplesOutStorageCondition (2)

If the SamplesOutStorageCondition is not set to AmbientStorage or Null, an error will be thrown:

If the SamplesOutStorageCondition is set to Disposal, an error will be thrown:

Possible Issues

Refresh Period

If a reference electrode is filled with an organic solvent reference solution, due to the glass frit structure of the reference electrode, the reference solution is likely to dry out in several weeks. Consider set the RecommendedRefreshPeriod field of such reference electrode models to a relatively short period of time, e. g. one or two weeks.

Last modified on Fri 21 Jan 2022 02:07:03