Test methods

Liquid-Phase and Dispersion Behavior

Separate incorporation, dispersion, separation,
and recovery

A powder entering a liquid can float, form persistent lumps, disperse into smaller units,
settle, build a network, or form a sediment that will not redisperse. These outcomes
require different tests. Choose the route by the preparation step, storage interval, and
product performance that matter.

Magnifying glass examining powder particles to identify observed process symptoms

Definition

What wetting, deagglomeration, physical stability, and redispersion each establish.

Clipboard checklist representing practical powder field guides

Selection factors

How liquid chemistry, concentration, preparation, time, and temperature shape the result.

Interconnected powder mechanisms showing relationships between underlying causes

Test methods

Choose among seven routes for preparing, characterizing, assessing, and recovering a suspension.

Powder measurement instrument and data display representing relevant measurements

Process relevance

Connect the evidence to mixing, formulation, storage, pumping, dosing, processing, and reuse.

Core concept

Preparation is not performance

Wetting allows liquid to contact and enter powder structures. Incorporation moves powder into the liquid. Deagglomeration separates associated particles under an imposed treatment. Dissolution transfers material into molecular or ionic solution. A powder disappearing from the surface does not prove that lumps have broken down or that the solid has dissolved.

Once prepared, a dispersion must be assessed over the relevant time and conditions. Sedimentation, optical profiles, accelerated separation, and rheology describe different aspects of its behavior. A suspension can settle yet redisperse well, or appear uniform while developing an unacceptable particle-size distribution or flow response.

PowderTechnology.info Insight

Define the required state before selecting the test: the as-used formulation, a process intermediate, or a deliberately diluted analytical preparation. Dilution, dispersant addition, and extra mixing may change the system that the measurement is intended to represent.

Key takeaway

Test the stage that controls the decision

Select wetting and incorporation trials for entry into the liquid, controlled deagglomeration for preparation response, sedimentation or optical profiling for physical change with time, centrifugation for a bounded accelerated comparison, rheology for flow and structure, and redispersion testing for recovery after aging. Preserve the relevant liquid composition, solids concentration, and preparation history. Neither a clear mixing endpoint, a single stability index, nor a high-acceleration result establishes complete dispersion quality or shelf life without independent evidence and application-specific acceptance criteria.

What controls it

Six decisions define a defensible dispersion test

<p>Start with the formulation and process question, then define a reproducible preparation and observation plan.</p>

Liquid chemistry

Control solvent composition, pH, ionic strength, dispersant dose, and dissolved species. Adsorption, dissolution, and particle interactions can change during testing.

Solids concentration

Use the process concentration where possible. Dilution changes collision rates, networks, optical response, and often sedimentation behavior.

Preparation history

Record addition order, mixing geometry, speed, duration, temperature, and rest time. Equal rpm does not imply equal energy input across mixers.

Time and temperature

Define the observation window, aging conditions, and sampling times. Temperature affects viscosity, interactions, dissolution, and evaporation.

Measurement suitability

Check optical range, density contrast, cell geometry, rheometer gap, wall slip, and whether the imposed field changes the structure.

Acceptance endpoint

Specify what must remain acceptable: uniformity, size distribution, viscosity, sediment volume, dose delivery, or recovery after remixing.

Selection and interpretation

Different dispersion tests answer different questions

<p>Compare results only after accounting for preparation, concentration, time, temperature, imposed motion, and the actual measured quantity.</p>

Engineering question

Primary route

Useful output

Critical boundary

Does powder enter the liquid reliably?Wetting and incorporationDefined incorporation endpoint and remaining lumpsSurface disappearance does not prove complete dispersion or dissolution
What treatment produces the required dispersed state?Controlled deagglomerationIndependent response versus treatmentAvoid confusing agglomerate breakup with primary-particle damage
What changes during ordinary storage?Gravitational sedimentationClarification, sediment development, and concentration distributionSediment volume alone does not establish redispersibility
Where and when does optical behavior change?Multiple light scatteringTransmission and backscatter profilesConcentration and particle changes can both affect the signal
How do formulations separate under acceleration?Analytical centrifugationSeparation profiles under a defined fieldAcceleration can change the mechanism and compress sediment
How does the suspension flow and recover?Suspension rheologyFlow curves and time-dependent or oscillatory responseControl slip, settling, geometry, and measurement history
Can the aged material return to an acceptable state?Controlled redispersionRecovery endpoint and residual cakeCloudiness alone is insufficient evidence of recovery

How to measure it

Select the method by the evidence the decision requires

The method sections below separate principle, sample state, preparation, output, limitation, disagreement, and decision use. Use the image selector above to jump directly to a method.

Test method 01

Wetting and incorporation

Measurement principle: Powder is added to a defined liquid under controlled mixing while entry into the liquid and persistent surface material are observed.

Suitable sample state: Representative powder and the actual or specified formulation liquid.

Sample preparation: Control powder addition rate and order, mass ratio, vessel, impeller, liquid level, agitation, temperature, and the endpoint definition. Record trapped air, floating material, and lumps.

Output and interpretation

Typical outputs: Incorporation time, residual floating fraction or visible lumps, and method-specific wetting descriptors.

Interpretation: Treat disappearance of surface powder as a defined incorporation endpoint. Confirm internal lump wetting, dissolution, or dispersion quality separately where required.

Principal limitation: The response combines surface wetting, air escape, powder structure, addition conditions, and hydrodynamics; it is not an intrinsic contact angle.

Decision and boundaries

Why results may disagree: A static sinking test, capillary penetration test, and agitated incorporation trial impose different boundaries and can rank powders differently.

Decision supported: Addition strategy, reconstitution conditions, and diagnosis of floating powder or persistent lumps.

Relevant standard: Use a documented formulation-specific procedure with an explicit endpoint; no universal incorporation-time limit applies across powders and liquids.

Compare surface and wettability methods

Test method 02

Controlled deagglomeration

Measurement principle: A defined mixing or dispersion treatment is applied in steps and its effect is measured independently.

Suitable sample state: A wetted suspension prepared at a stated solids content and liquid composition.

Sample preparation: Specify mixer or disperser geometry, speed, time, temperature control, sample volume, addition sequence, and sampling. Track power or energy where meaningfully measured.

Output and interpretation

Typical outputs: Particle-size or microscopy response versus treatment, residual agglomerates, and changes in rheology or product performance.

Interpretation: Choose the preparation endpoint that represents the intended process state. A size plateau alone can conceal competing breakup and reagglomeration or limited measurement sensitivity.

Principal limitation: Excess treatment can fracture primary particles, heat the sample, promote dissolution, or introduce wear debris. Rotor speed alone is not a transferable measure of shear or energy.

Decision and boundaries

Why results may disagree: Different geometries, residence times, dilution steps, and analysis settings can produce different apparent dispersion endpoints.

Decision supported: Dispersion-protocol development, comparison of mixing treatments, and identification of insufficient or excessive processing.

Relevant standard: Use a validated preparation protocol paired with an appropriate independent measurement; distinguish process-representative dispersion from preparation intended to resolve primary particles.

Choose the particle-size verification route

Test method 03

Gravitational sedimentation

Measurement principle: A suspension is held under gravity while concentration distribution, interfaces, or sediment development are followed with time.

Suitable sample state: A representative suspension in a compatible observation vessel.

Sample preparation: Control preparation, concentration, vessel dimensions, fill height, closure, temperature, vibration, observation times, and any sampling disturbance.

Output and interpretation

Typical outputs: Interface position, settling or clarification rate, sediment height or volume, and time-dependent concentration or turbidity.

Interpretation: Interpret sediment formation together with supernatant quality and later redispersion. Rapid settling into a loose sediment and slow formation of a dense cake are different outcomes.

Principal limitation: Stokes-based size inference requires suitable dilute, isolated-particle, creeping-flow assumptions, known fluid and particle properties, and negligible wall effects. Concentrated, flocculated, or networked suspensions need other interpretation.

Decision and boundaries

Why results may disagree: Particle interactions, density contrast, viscosity, vessel size, and sample history can alter settling even when particle-size results look similar.

Decision supported: Storage comparison, visible separation diagnosis, and selection of aging conditions for subsequent recovery testing.

Relevant standard: ISO/TR 13097:2013 provides guidance on dispersion-stability characterization; use a documented gravity-storage procedure and product-specific acceptance criteria.

Connect the result to sedimentation

Test method 04

Multiple light scattering

Measurement principle: Transmission and backscattering profiles are recorded along a sample to track physical changes with time.

Suitable sample state: A dispersion compatible with the instrument optics, sample cell, and validated concentration range.

Sample preparation: Control concentration, liquid composition, sample preparation, cell cleanliness and path length, temperature, scan interval, and analysis region. Avoid bubbles and unintended disturbance.

Output and interpretation

Typical outputs: Transmission and backscattering profiles, migration-front changes, and instrument-specific comparative indices.

Interpretation: Use the position and evolution of signal changes to investigate migration and changes in particle or aggregate populations. Confirm the mechanism with complementary evidence.

Principal limitation: Optical response depends on both concentration and scattering properties, including particle size and refractive-index contrast. A signal change does not uniquely identify a destabilization mechanism.

Decision and boundaries

Why results may disagree: Different wavelengths, optical ranges, scan programs, regions, and index calculations can yield different rankings. Compare indices only under a defined common protocol.

Decision supported: Early detection of physical change and comparative formulation screening at a relevant concentration.

Relevant standard: ISO/TR 13097:2013 supplies general stability guidance, not a universal optical-index threshold. Follow the validated instrument procedure.

Interpret migration in context

Test method 05

Analytical centrifugation

Measurement principle: Optical profiles are monitored during centrifugation to follow separation under a defined acceleration field.

Suitable sample state: A suspension suitable for the rotor cells, optical range, and intended analytical model.

Sample preparation: Report rotor speed, radial position or acceleration range, temperature, cell and optical path, loading, concentration, run program, and preparation history.

Output and interpretation

Typical outputs: Space- and time-resolved transmission profiles, separation velocities, and method-specific comparative separation descriptors.

Interpretation: Use accelerated results to compare formulations within a validated protocol. Relate rankings to ordinary storage data before making a storage-performance claim.

Principal limitation: Higher acceleration can alter networks, compress sediment, or activate separation that differs from storage under gravity. Run time multiplied by acceleration is not a general shelf-life conversion.

Decision and boundaries

Why results may disagree: Acceleration, cell geometry, concentration, density contrast, viscosity, and model assumptions affect the result and may change formulation rankings.

Decision supported: Accelerated separation screening and investigation of migration or sediment consolidation.

Relevant standard: ISO 13318-1:2024 addresses centrifugal liquid sedimentation for particle-size analysis under its stated scope, including dilute conditions. It does not establish a universal concentrated-dispersion stability or shelf-life test.

Separate particle sizing from stability assessment

Test method 06

Suspension rheology

Measurement principle: A controlled deformation is applied while stress or strain response is measured using a suitable rheometer geometry.

Suitable sample state: A representative suspension that fits the geometry and remains sufficiently controlled during measurement.

Sample preparation: Specify geometry and gap, particle-size suitability, temperature, preshear, rest period, loading, evaporation control, and the stress or rate sequence. Check wall slip and settling.

Output and interpretation

Typical outputs: Viscosity versus shear rate, stress response, time-dependent recovery, and, with suitable oscillatory testing, storage and loss moduli.

Interpretation: Relate the measurement range to pumping, mixing, dosing, or resting behavior. Yield values depend on the procedure; distinguish shear thinning from time-dependent structural change.

Principal limitation: Wall slip, particle migration, settling, gap restrictions, inertia, and instrument resolution can dominate apparent behavior. A single viscosity value cannot describe the full suspension response.

Decision and boundaries

Why results may disagree: Different preshear, rest periods, ramp directions, geometry surfaces, and fit models may produce different viscosity or yield estimates.

Decision supported: Pumping and dosing conditions, formulation structure, recovery after shear, and consistency assessment.

Relevant standard: ISO 3219-2:2021 gives general principles of rotational and oscillatory rheometry. Use a suspension-appropriate protocol; it does not supply one universal yield-stress procedure.

Check recovery after storage

Test method 07

Controlled redispersion

Measurement principle: An aged suspension is remixed under a defined treatment and recovery is assessed against a stated endpoint.

Suitable sample state: An aged suspension with documented storage conditions and a matched fresh reference.

Sample preparation: Control aging time, temperature, orientation, container, fill and headspace, mixing motion, rate and duration, and sampling positions. Define residual-cake and uniformity checks.

Output and interpretation

Typical outputs: Mixing time or cycle count to a defined recovery endpoint, residual sediment, and recovered concentration uniformity or particle-size and rheology response.

Interpretation: Verify recovery with appropriate measurements. A cloudy appearance alone does not establish uniform concentration, complete cake breakup, or restoration of product performance.

Principal limitation: Cycle count and time are method-specific rather than universal energy measures. Aggressive remixing can create a new state by breaking primary particles.

Decision and boundaries

Why results may disagree: Aging history, sediment compaction, container geometry, mixing mode, and endpoint sensitivity can change the apparent ease of recovery.

Decision supported: Package-use instructions, recovery after storage, formulation comparison, and evaluation of irreversible sediment formation.

Relevant standard: Use a documented product-specific aging and remixing procedure with independent recovery criteria; no universal redispersion limit applies to all suspensions.

Compare the recovered rheology

Conditional routes

When the suspension test needs a companion method

Add an orthogonal measurement when the engineering question extends beyond physical dispersion behavior.

Surface chemistry or charge is the uncertainty

Use contact-angle, capillary-penetration, or electrokinetic methods when the question concerns interfaces. These do not replace a formulation-level dispersion trial. Compare surface methods.

The measured particle size changes after preparation

Check sampling, dilution, dispersion treatment, dissolution, and the measurement model before assigning the change to the original powder. Compare sizing routes.

Dissolution is the actual endpoint

Use a suitable dissolved-concentration assay and validated phase-separation or sampling procedure. Turbidity loss or disappearance of visible powder is not by itself a dissolution measurement.

Chemical or biological change controls storage

Add appropriate chemical, microbiological, or application-specific testing. Physical separation measurements alone do not establish chemical stability, microbiological quality, or usable shelf life.

Process relevance

Connect the evidence to the operating step

A useful test links a controlled material state to an observable operating or product requirement.

01

Powder addition

Compare addition order and rate under realistic mixing to reduce floating material and persistent lumps.

02

Dispersion processing

Set treatment limits using independent evidence of breakup, temperature rise, and unwanted particle damage.

03

Formulation screening

Compare physical change using common preparation, concentration, temperature, and observation windows.

04

Storage and transport

Combine ordinary aging with bounded accelerated screening and a check on sediment recovery.

05

Pumping and dosing

Measure flow and recovery over the relevant operating range and check concentration uniformity during withdrawal.

06

Reuse and reconstitution

Confirm that the prescribed remixing restores acceptable material rather than simply making sediment less visible.

Technical FAQ

Common questions about dispersion testing

Keep preparation, physical stability, and recovery distinct when comparing results.

No. Liquid entry and disappearance of surface powder do not prove that agglomerates have broken down, that concentration is uniform, or that the solid has dissolved. Verify the required endpoint independently.
No. Dilution can change interactions, networks, viscosity, settling, and optical behavior. Use the relevant concentration where the method permits it, and document any necessary dilution and its effect on interpretation.
No. Acceptance depends on the product requirement and time window. A loose sediment that redistributes easily may be acceptable, while a compact cake or nonuniform delivered dose may not be.
Not by itself. Such indices depend on the instrument and analysis protocol. Establish their relevance against defined acceptance criteria and storage observations for the formulation.
Not in general. Acceleration can change particle interactions, networks, and sediment compaction. Any conversion or prediction needs a validated model and comparison with ordinary storage behavior.
Define aging and remixing conditions, then check the relevant recovery endpoint, such as concentration uniformity, residual cake, particle size, rheology, or delivered performance. Visual cloudiness alone is insufficient.

Go deeper

Continue into wetting and dispersion

These published PTI articles provide processing and application context. Use the scoped references below for the technical basis of method selection.

Featured image for Powder Wettability: Why Powders Float, Clump, or Disperse

Powder Wettability: Why Powders Float, Clump, or Disperse

Explore the first contact between powder and liquid and the causes of floating material and persistent lumps.

Read the article

Featured image for Dispersion in Powder Processing and Lab Testing

Dispersion in Powder Processing and Lab Testing

Read the broader processing context for dispersion and laboratory preparation.

Read the article

Featured image for Inside Perspective of Powder Wettability in the Food and Feed Industries

Inside Perspective of Powder Wettability in the Food and Feed Industries

Connect wetting behavior with reconstitution and ingredient handling in food and feed applications.

Read the article

Technical basis / sources

Sources and scope boundaries

Select the edition and scope appropriate to the measurement. Guidance documents and instrument descriptions do not create universal pass/fail limits.

  • ISO/TR 13097:2013: guidance for characterizing dispersion stability; it does not prescribe one universal stability index or acceptance threshold.
  • ISO 13318-1:2024: centrifugal liquid sedimentation for particle-size analysis, including its dilute-system assumptions; distinguish this scope from concentrated-formulation stability screening.
  • ISO 3219-2:2021: general principles of rotational and oscillatory rheometry; supplement these with suspension-specific geometry and history controls.
  • Microtrac static multiple light scattering and LUMiSizer analytical centrifugation: instrument-principle references, not universal shelf-life validation procedures.
  • Wetting, deagglomeration, gravity storage, and redispersion trials require documented sample preparation, operating conditions, replicate plans, and independently defined endpoints suited to the product.

Need the measurement, not just the guidance?

If the uncertainty concerns powder incorporation, dispersion treatment, separation, suspension flow, or recovery after storage, define the relevant formulation state and process conditions before commissioning tests. Agree the preparation history, liquid composition, solids concentration, observation period, and interpretation boundaries with the laboratory. PTI works closely with Delft Solids Solutions, a contract research organization specializing in the physical behavior of powders and granules. Contact Delft Solids Solutions.

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