ASTM D8539-23

Standard Guide for Measurement of Polyolefin Properties Using TD-NMR Relaxometry

SIGNIFICANCE AND USE
5.1 This guide is intended to assist users how to determine polymer properties in polyolefins related to their morphology (2) using TD-NMR Relaxometry, for example, Xylene Solubles (XS) content in polypropylene (PP).  
5.2 The advantage of using TD-NMR Relaxometry lies in the fact that the method is rapid, non-destructive, cost effective, safe for the operator, environmentally friendly, and less dependent on operator consistency than traditional methods.  
5.3 These polymer properties are measured for Quality Assurance (QA), Quality Control (QC) (7) and process control, for example, certificates of analysis (CoA) or optimization of the reaction process (6). These properties are key indicators of performance characteristics and are therefore important in compounding and manufacturing of plastic products.  
5.3.1 This guide is applicable in a laboratory environment, continuous inspection as a quality control or as a research tool. It is also appropriate for use in commercial processes used to produce polyethylene and polypropylene.  
5.4 TD-NMR Relaxometry can measure crystallinity content and relaxation rates directly (4), (5). Polyolefin properties used in industry that are correlated with crystallinity can be quantified. In these cases, a calibration is necessary.  
5.5 As a secondary technique, results achieved by different TD-NMR Relaxometry systems, even from the same vendor, in different laboratories are not necessarily comparable and may result in biases. Therefore, the user is advised to perform measurement validation.
SCOPE
1.1 This guide is intended to provide suggested approaches and criteria for the determination of polyolefin properties via time-domain Nuclear Magnetic Resonance (TD-NMR) Relaxometry. Though any crystallinity or morphology related property can be determined using this method (1), (2)2, the focus of this guide is on the prediction of Xylene Solubles content for polypropylene and density (3) for polyethylene as these are the most commonly specified properties for polyolefin manufacturers. Please note that other properties such as flexural modulus, Izod, Charpy, intrinsic viscosity, decalin/hexane solubles and others can be determined as well.  
1.2 High-Level Purpose—The purpose of this guide includes:
(1) educating new users on the use of TD-NMR Relaxometry to determine properties of polyolefins in manufacturing plants and laboratories;
(2) providing a standard terminology that can be used by different vendors and end users;
(3) establishing minimum requirements for apparatus, data acquisition, analysis, calibration and validation;
(4) providing guidance for the specification, evaluation, cost justification, implementation, project management, training, and documentation of TD-NMR Relaxometers; and
(5) providing a functional requirements checklist for TD-NMR Relaxometers for use in polyolefin plants and laboratories that can be integrated with existing systems.  
1.3 Audience—This guide has been created with the needs of the following stakeholders in mind:
(1) end users of TD-NMR Relaxometers for use in polyolefin plants and laboratories,
(2) implementers of TD-NMR Relaxometers for use in polyolefin plants and laboratories,
(3) quality personnel,
(4) information technology personnel,
(5) vendors of TD-NMR Relaxometers for use in polyolefin plants and laboratories,
(6) individuals who approve funding of TD-NMR Relaxometers for use in polyolefin plants and laboratories,
(7) applications support specialists for TD-NMR Relaxometers used in polyolefin plants and laboratories, and
(8) software test/validation specialists.  
1.4 Information contained in this guide will benefit a broad audience of people who interact with a TD-NMR Relaxometer used in polyolefin plants and laboratories. New users can use this guide to understand the purpose and functions of TD-NMR Relaxometers for use in polyolefin plants and laboratories as well as the int...

General Information

• Status: Published
• Publication Date: 31-Oct-2023
• Technical Committee: D20 - Plastics
• Drafting Committee: D20.70 - Analytical Methods

Standards Content (Sample)

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.
Designation: D8539 − 23
Standard Guide for
Measurement of Polyolefin Properties Using TD-NMR
1
Relaxometry
This standard is issued under the fixed designation D8539; 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 (4) information technology personnel,
(5) vendors of TD-NMR Relaxometers for use in poly-
1.1 This guide is intended to provide suggested approaches
olefin plants and laboratories,
and criteria for the determination of polyolefin properties via
(6) individuals who approve funding of TD-NMR Relax-
time-domain Nuclear Magnetic Resonance (TD-NMR) Relax-
ometers for use in polyolefin plants and laboratories,
ometry. Though any crystallinity or morphology related prop-
2
(7) applications support specialists for TD-NMR Relaxom-
erty can be determined using this method (1), (2) , the focus of
eters used in polyolefin plants and laboratories, and
this guide is on the prediction of Xylene Solubles content for
(8) software test/validation specialists.
polypropylene and density (3) for polyethylene as these are the
most commonly specified properties for polyolefin manufac-
1.4 Information contained in this guide will benefit a broad
turers. Please note that other properties such as flexural
audience of people who interact with a TD-NMR Relaxometer
modulus, Izod, Charpy, intrinsic viscosity, decalin/hexane
used in polyolefin plants and laboratories. New users can use
solubles and others can be determined as well.
this guide to understand the purpose and functions of TD-NMR
1.2 High-Level Purpose—The purpose of this guide in- Relaxometers for use in polyolefin plants and laboratories as
cludes: well as the interactions between these tools with external
(1) educating new users on the use of TD-NMR Relaxom- systems. The guide might also help prospective users in
etry to determine properties of polyolefins in manufacturing understanding terminology, configurations, features, design,
plants and laboratories; benefits, and costs of these analyzers. Individuals who are
(2) providing a standard terminology that can be used by purchasing TD-NMR Relaxometers for use in polyolefin plants
different vendors and end users;
and laboratories may also use this guide to identify functions
(3) establishing minimum requirements for apparatus, data
that are recommended for specific laboratory environments.
acquisition, analysis, calibration and validation;
Research and development staff of different commercial labo-
(4) providing guidance for the specification, evaluation,
ratory informatics system vendors may use the guide as a tool
cost justification, implementation, project management,
to evaluate, identify, and potentially improve the capabilities of
training, and documentation of TD-NMR Relaxometers; and
their products. The vendors’ sales staff may use the guide to
(5) providing a functional requirements checklist for TD-
represent functions of their laboratory informatics products to
NMR Relaxometers for use in polyolefin plants and laborato-
prospective customers in more generic and product-neutral
ries that can be integrated with existing systems.
terms.
1.3 Audience—This guide has been created with the needs
1.5 This standard does not purport to address all of the
of the following stakeholders in mind:
safety concerns, if any, associated with its use. It is the
(1) end users of TD-NMR Relaxometers for use in poly-
responsibility of the user of this standard to establish appro-
olefin plants and laboratories,
priate safety, health, and environmental practices and deter-
(2) implementers of TD-NMR Relaxometers for use in
mine the applicability of regulatory limitations prior to use.
polyolefin plants and laboratories,
NOTE 1—There is no known ISO equivalent to this standard guide.
(3) quality personnel,
1.6 This international standard was developed in accor-
1
dance with internationally recognized principles on standard-
This test method is under the jurisdiction of ASTM Committee D20 on Plastics
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods.
ization established in the Decision on Principles for the
Current edition approved Nov. 1, 2023. Published November 2023. DOI:
Development of International Standards, Guides and Recom-
10.1520/D8539-23
2 mendations issued by the World Trade Organization Technical
The boldface numbers in parentheses refer to a list of references at the end of
this standard. Barriers to Trade (TBT) Committee.
Copyright ©
...