ISO/TS 23361:2024
(Main)Nanotechnologies — Crystallinity of cellulose nanomaterials by powder X-ray diffraction (Rietveld analysis)
Nanotechnologies — Crystallinity of cellulose nanomaterials by powder X-ray diffraction (Rietveld analysis)
This document specifies the determination of the bulk crystallinity (crystalline contribution relative to the total crystalline and amorphous contributions in the material) of cellulose nanomaterials using powder X-ray diffraction followed by deconvolution of the diffraction patterns based on Rietveld analysis. It is applicable to all types of cellulose nanomaterials, assuming a representative sample.
Nanotechnologies — Cristallinité des nanomatériaux à base de cellulose par diffraction aux rayons X sur poudre (analyse de Ruland-Rietveld)
General Information
Standards Content (Sample)
Technical
Specification
ISO/TS 23361
First edition
Nanotechnologies — Crystallinity of
2024-10
cellulose nanomaterials by powder
X-ray diffraction (Rietveld analysis)
Nanotechnologies — Cristallinité des nanomatériaux à base de
cellulose par diffraction aux rayons X sur poudre (analyse de
Ruland-Rietveld)
Reference number
© ISO 2024
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ii
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
3.1 Core nanotechnology terms related to cellulose nanomaterials .1
3.2 Non-nanotechnology terms related to cellulose nanomaterials .2
3.3 Terms specific to cellulose nanomaterials.2
4 Principle . 4
5 Sample preparation . 5
5.1 General considerations.5
5.2 Preparation of samples from powders .5
6 Instrument and software requirements . 6
6.1 Diffractometer .6
6.2 Software .6
6.3 Crystallographic information files .6
7 Data collection . . 6
8 Data processing and analysis . 7
8.1 General considerations.7
8.2 Modelling procedure .8
9 Uncertainty . 10
10 Test report .11
Annex A (informative) Results of interlaboratory comparison .12
Bibliography .21
iii
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
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The procedures used to develop this document and those intended for its further maintenance are described
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This document was prepared by Technical Committee ISO/TC 229, Nanotechnologies.
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iv
Introduction
Cellulose nanomaterials (CNM) are a family of emerging bioproducts with significant commercial impact. Their
production from abundant cellulose sources such as wood pulps makes them a candidate for use as a potentially
non-toxic, biodegradable and sustainable nanomaterial for a wide range of applications, including those that
currently use petroleum-based components. Several types of CNM are currently produced in a number of
countries on pilot, pre-commercial or commercial scales. Realizing the full potential of these materials requires
standard methods for characterization of a range of material properties, including crystallinity. Crystallinity
is an indication of material quality, success of processing, and degradation of the material during processing,
which can affect performance for various applications, particularly for use in nanocomposites. Crystallinity
is also important for distinguishing between CNC grades and products and ensuring batch control and
repeatability, and can provide information on the cellulose source and production method.
Crystallinity of CNM is defined as the fraction of the material composed of crystallites. There are several
approaches for measuring crystallinity of materials, including powder X-ray diffraction, differential
scanning calorimetry and solid-state nuclear magnetic resonance. Each of these techniques obviously has
its merits and limitations. Use of crystallinity for quality control purposes for CNM production and further
processing requires a measurement method that can be quickly, routinely and reproducibly implemented
and that is easily accessible and can be run in most laboratories with the same level of proficiency. Powder
X-ray diffraction addresses these criteria. This technical specification describes the measurement of CNM
crystallinity by powder X-ray diffraction using deconvolution of the diffraction pattern based on Rietveld
analysis. The Rietveld method allows a diffraction profile to be modelled based on known diffraction peaks
for a specific crystallographic structure by attempting to minimize the difference between the calculated
and observed patterns by the least-squares method.
The Rietveld method requires that the powder diffraction pattern be representative of the sample, which
requires careful sample preparation and assumes a randomly oriented sample. The instrument configuration
and detector sensitivity are also important. This document provides guidance on both sample preparation
and instrument configuration and operating parameters. The method is applicable to all types of CNM,
including cellulose nanocrystals, cellulose nanofibrils and cellulose filaments.
v
Technical Specification ISO/TS 23361:2024(en)
Nanotechnologies — Crystallinity of cellulose nanomaterials
by powder X-ray diffraction (Rietveld analysis)
1 Scope
This document specifies the determination of the bulk crystallinity (crystalline contribution relative to the
total crystalline and amorphous contributions in the material) of cellulose nanomaterials using powder
X-ray diffraction followed by deconvolution of the diffraction patterns based on Rietveld analysis. It is
applicable to all types of cellulose nanomaterials, assuming a representative sample.
2 Normative references
There are no normative references in this document.
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at https:// www .electropedia .org/
3.1 Core nanotechnology terms related to cellulose nanomaterials
3.1.1
nanoscale
length range approximately from 1 nm to 100 nm
[SOURCE: ISO 80004-1:2023, 3.1.1]
3.1.2
nanomaterial
material with any external dimension in the nanoscale (3.1.1) or having internal structure or surface
structure in the nanoscale
Note 1 to entry: Certain types of nanomaterials include engineered, manufactured and incidental nanomaterials.
Note 2 to entry: The nanoform of a material is a nanomaterial.
[SOURCE: ISO 80004-1:2023, 3.14, modified — Note 1 to entry has been adapted to this document.]
3.1.3
nano-object
discrete piece of material with one, two or three external dimensions in the nanoscale (3.1.1)
[SOURCE: ISO 80004-1:2023, 3.1.5]
3.1.4
nanofibre
nano-object (3.1.3) with two similar external dimensions in the nanoscale (3.1.1) and the third dimension
significantly larger
Note 1 to entry: The largest external dimension is not necessarily in the nanoscale.
[SOURCE: ISO 80004-1:2023, 3.3.5]
3.1.5
nanocrystal
nano-object (3.1.3) with a crystalline structure
[SOURCE: ISO 80004-1:2023, 3.1.15]
3.2 Non-nanotechnology terms related to cellulose nanomaterials
3.2.1
crystalline
having a solid structure with a three-dimensional arrangement of ions, molecules, or atoms with long
range order
[SOURCE: ISO/TS 20477:2023, 3.2.1]
3.2.2
amorphous
regions within a polymeric material that, on the basis of X-ray diffraction or other suitable techniques, do
not show any evidence of crystalline structure
[SOURCE: ISO 472:2013, 2.50]
3.2.3
paracrystalline
having short and medium range ordered lattice structure and lacking long range order in at least one
direction; in the intermediate state between crystalline (3.2.1) and amorphous (3.2.2)
[SOURCE: ISO/TS 20477:2023, 3.2.2]
3.2.4
cellulose
linear polymeric chains of β (1→4) linked D-glucopyranose units
[SOURCE: ISO/TS 20477:2023, 3.2.3]
3.2.5
elementary fibril
structure, originating from a single terminal enzyme complex, having a configuration of cellulose chains
specific to each cellulose-producing plant, animal, algal and bacterial species
[SOURCE: ISO/TS 20477:2023, 3.2.4]
3.3 Terms specific to cellulose nanomaterials
3.3.1
cel
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