ASTM E3427-24 Standard Guide for Measuring Intensity,Polydispersity,Size,Zeta Potential,Molecular Weight,and Concentration of Nanoparticles in Liquid Suspension Using Laser-Amplified Detection/Power Spectrum Analysis (LAD/PSA) Technology

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Designation: E3427 −24
Standard Guide for
Measuring Intensity, Polydispersity, Size, Zeta Potential,
Molecular Weight, and Concentration of Nanoparticles in
Liquid Suspension Using Laser-Ampliﬁed Detection/Power
Spectrum Analysis (LAD/PSA) Technology
1
This standard is issued under the ﬁxed designation E3427; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 The technology, laser-ampliﬁed detection/power spec-
trum analysis (LAD/PSA), is available in three different
platforms, which will be designated as Platforms A, B, and C.
1.1.1 Platform A—This is a solid-state probe conﬁguration
that serves as the optical bench in each of the platforms. It
consists of an optical ﬁber coupler with a y-beam splitter that
directs the scattered light signal from the nanoparticles at 180°
back to a photodiode detector. The sensing end of the probe can
be immersed in a suspension or positioned to measure one drop
of a sample on top of the sensing surface.
1.1.2 Platform B—The same probe is mounted in a case,
positioned horizontally, to detect the signal from either a
disposable or permanent cuvette.
1.1.3 Platform C—Two probes are mounted in a case,
horizontally, at opposite sides of a permanent sample cell. Both
size distribution and zeta potential can be measured in this
conﬁguration.
1.2 The laser beam travelling through the probe measuring
the scattered light from the sample of nanoparticles, in all three
platforms, is partially reﬂected back to the same photodiode
detector, and the high optical power of the laser is added to the
low optical power of the scattered light signal. The interference
(mixing or beating) of those two signals is known as hetero-
dyne beating. The resulting high-power detected signal pro-
vides the highest signal-to-noise ratio among dynamic light-
scattering (DLS) technologies.
1.3 This combined, ampliﬁed, optical signal is converted
with a Fast Fourier transform (FFT) into a frequency power
spectrum, then into a logarithmic power spectrum that is
deconvolved into number and volume size distributions. The
mean intensity, polydispersity, number and volume size
distributions, concentration, and molecular weight can be
reported in all platforms, plus zeta potential on Platform C.
1.4 This technology is capable of measuring nanoparticles
in a size range from 2.0 nanometres (nm) to 10 micrometres
(µm), at concentrations in a suspending liquid medium up to
40 % cc ⁄mL for all parameters given in 1.3.
1.5 Units—The values stated in SI units are to be regarded
as the standard. No other units of measurement are included in
this standard.
1.6 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
1.7 This international standard was developed in accor-
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
2
E1817 Practice for Controlling Quality of Radiological Ex-
amination by Using Representative Quality Indicators
(RQIs)
E2456 Terminology Relating to Nanotechnology
E2490 Guide for Measurement of Particle Size Distribution
of Nanomaterials in Suspension by Photon Correlation
Spectroscopy (PCS)
E2834 Guide for Measurement of Particle Size Distribution
of Nanomaterials in Suspension by Nanoparticle Tracking
Analysis (NTA)
E3247 Test Method for Measuring the Size of Nanoparticles
1
This guide is under the jurisdiction of ASTM Committee E29 on Particle and
Spray Characterization and is the direct responsibility of Subcommittee E29.02 on
Non-Sieving Methods.
Current edition approved Feb. 1, 2024. Published February 2024. DOI: 10.1520/
E3427-24.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
1

in Aqueous Media Using Dynamic Light Scattering
2.2 ISO Standards:
3
ISO 14488 Particulate Material—Sampling and Sample
Splitting for the Determination of Particulate Properties
ISO 22412 Particle Size Analysis—Dynamic Light Scatter-
ing (DLS)
3. Terminology
3.1 Deﬁnitions—For deﬁnitions of terms pertaining to this
guide not otherwise listed in 3.2, reference should be made to
ISO 22412, Guides E2490 and E2834, and Test Method E3247.
3.2 Deﬁnitions of Terms Speciﬁc to This Standard:
3.2.1 deconvolution, n—iterative computational technique
that calculates an estimate of the answer to a problem.
3.2.1.1 Discussion—The error between the problem and the
estimate is calculated and the estimate is reﬁned. The process
is repeated until the error is minimized to a desired minimal
value.
3.2.2 Fast Fourier transform, FFT, n—algorithm that con-
verts a signal from the amplitude/time domain to the
amplitude/frequency domain.
3.2.3 ﬁber optic coupler, n—ﬁber optic device capable of
combining two or more inputs into a single output and also
dividing a single input into two or more outputs.
3.2.4 heterodyne (reference beating), adj—heterodyne de-
tection is the mixing of scattered light from nanoparticles with
a reference light beam from the same source, which is a laser
in this technology (refer to heterodyne diagram in Fig. 1).
3.2.4.1 Discussion—Sinusoidal electromagnetic waves are
generated, as related to dynamic light scattering (DLS), from
each nanoparticle in the scattering region of the incident laser
signal. The intensity of the scattered light from each nanopar-
ticle is added to the intensity of the laser reference beam of
much greater optical power than the optical power of the
scattered light from the nanoparticles.
3.2.5 homodyne (self-beating), adj—sinusoidal electromag-
netic waves are generated, as related to DLS, from all the
different pairs of nanoparticles in the scattering region of the
incident laser signal representing the sum of the scattered light
intensity for each pair added together (refer to homodyne
diagram in Fig. 1).
3.2.6 y-splitter, n—location in a ﬁber optic coupler where a
single beam is divided into two beams and where two beams
are combined into one.
3.3 Acronyms:
3.3.1 CWV—constant water volume
3.3.2 DI—deionized
3.3.3 DLS—dynamic light scattering
3.3.4 FPS—frequency power spectrum
3.3.5 IPA—isopropyl alcohol
3.3.6 LAD/PSA—laser-ampliﬁed detection/power spectrum
analysis
3.3.7 LI—loading index
3.3.8 MI—mean intensity
3.3.9 MW—molecular weight
3.3.10 NTA—nanoparticle tracking analysis
3.3.11 PCS—photon correlation spectroscopy
3.3.12 PI—polydispersity index
3.3.13 PSA—power spectrum analysis
3.3.14 PSD—power spectrum distribution
3.3.15 QLS—quasi-elastic light scattering
3.3.16 RI—refractive index
3.3.17 RRI—relative refractive index
3
Available from International Organization for Standardization (ISO), ISO
Central Secretariat, Chemin de Blandonnet 8, CP 401, 1214 Vernier, Geneva,
Switzerland, https://www.iso.org.
FIG. 1 Comparison Diagrams of Homodyne and Heterodyne Detection
E3427 − 24
2

4. Signiﬁcance and Use

4.1 In this guide, the conditions, measurement apparatus,

and procedures for measuring several characteristics of nan-

oparticle properties on three different instrument platforms

using laser-ampliﬁed detection/power spectrum analysis

(LAD/PSA) technology are described. This is a more recently

developed technology, commercialized in 1990, than the older

technology known as either photon correlation spectroscopy

(PCS) or quasi-elastic light scattering (QLS)—those titles are

interchangeable—developed ﬁrst in 1961. Nanoparticle track-

ing analysis (NTA) is the most recent DLS technology to be

commercialized. All three of these technologies fall under the

broader category of DLS, based on the “dynamic” movement

of the measured nanoparticles under Brownian motion.

4.2 DLS in the lower end of the nanometre size range

becomes progressively more difficult as the particle optical

scattering coefficients drop sharply, reducing the scattered light

intensity. The advantage of the heterodyne detection mode over

the homodyne detection mode, especially at the low end of the

nanometre range, will be explained.

4.3 The LAD/PSA technology will be described and the

major differences between it and the PCS-QLS and NTA

technologies will be made clear. For thorough discussions of

PCS-QLS, refer to Guide E2490, Test Method E3247, and ISO

22412 Annex Section A.1. For a thorough discussion of

nanoparticle tracking analysis (NTA), refer to Guide E2834.

For detailed information on laser-ampliﬁed detection/

frequency power spectrum (LAD/FPS) technology, refer to

ISO 22412 Annex Section A.2. General information on particle

characterization practices can be found in Practice E1817, and

nanotechnology terminology is given in Terminology E2456.

Detailed information on sampling for particle characterization

can be found in ISO 14488.

5. Procedure

5.1 Laser-Ampliﬁed Detection (LAD)—In this guide, the

differences among three different instrument Platforms, A, B,

and C, will be made clear using this type of detection and

subsequent analysis. This type of particle measurement tech-

nology is used to measure, and report mean intensity, polydis-

persity index (PI), number and volume size distributions,

concentration, molecular weight, and zeta potential of nanopar-

ticles in a liquid undergoing Brownian motion. Brownian

motion refers to the random movement displayed by small

particles that are suspended in ﬂuids being struck by the

molecules in solution as a function of the temperature and

viscosity of the ﬂuid. This motion is a result of the collisions of

the particles with the random movement of the molecules in the

ﬂuid. LAD uses heterodyne detection. PCS-QLS uses homo-

dyne detection. PCS-QLS uses time-based autocorrelation to

process the detected homodyne signal. LAD/PSA uses power

spectrum analysis to process the detected heterodyne signal.

5.1.1 Platform A—This is a solid-state probe conﬁguration

that serves as the optical bench in all three platforms. This

platform measures all parameters mentioned in 5.1 except zeta

potential. It consists of an optical ﬁber coupler with a y-splitter

enclosed in a stainless-steel cylindrical casing (see Fig. 2). A

laser signal travels through a Grin lens that maintains the

spatial separation of the nanoparticles and then through a

sapphire window that has a high reﬂectance. The nanoparticles

scatter light back to the probe window at 180° at frequencies in

the thousands of Hertz (audible) range compared to the

constant laser reference frequency in the range of about 14

Terahertz (4.61 × 10

Hz). Computers do not scan at a high

enough speed to detect the frequency shifts at these

frequencies, so the high-frequency (laser) component is sub-

tracted from the combined frequencies and that allows the

successful detection of the low (scatter) frequency shift signals.

The interference of a high-power, unchanging, reference signal

(laser beam) with a lower-power, changing, measured signal

(the scattered light) is heterodyne detection. These two sinu-

soidal wave forms interfere with each other, resulting in a beat

signal with an optical power that is the sum of the weak

scattered light signal and the high power of the laser signal. As

light scatters from the moving nanoparticles, this motion

imparts a randomness to the phase of the scattered light, such

that when the scattered light from each particle is added to the

constant frequency laser reference beam, there will be a

changing constructive or destructive interference. This leads to

time-dependent ﬂuctuations in the intensity of the scattered

light. When no reference signal is used, the scattered light from

all pairs of particles interfering with each other is summed and

so is the homodyne detection with a much lower optical power

FIG. 2 LAD/PSA Heterodyne Detection Probe

E3427 − 24

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ASTM E3427-2024 Standard Guide for Measuring Intensity,Polydispersity,Size,Zeta Potential,Molecular Weight,and Concentration of Nanoparticles in Liquid Suspension Using Laser-Amplified Detection/Power Spectrum Analysis (LAD/PSA) Technology

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ASTM E3427-24 Standard Guide for Measuring Intensity,Polydispersity,Size,Zeta Potential,Molecular Weight,and Concentration of Nanoparticles in Liquid Suspension Using Laser-Amplified Detection/Power Spectrum Analysis (LAD/PSA) Technology

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