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ASTM D8402-23

(Practice)

Standard Practice for Development of Microplastic Reference Samples for Calibration and Proficiency Evaluation in All Types of Water Matrices with High to Low Levels of Suspended Solids

Standard Practice for Development of Microplastic Reference Samples for Calibration and Proficiency Evaluation in All Types of Water Matrices with High to Low Levels of Suspended Solids

SIGNIFICANCE AND USE
5.1 These procedures can be used to generate microplastic particles as a simulation of microplastic particles found in the natural environment. Suitable uses may include evaluation of microplastic detection and imaging methods. Use of reference samples will support estimation of ambient and flux concentrations in drinking water, wastewater and natural environments, investigations of microplastic particle degradation, and ingestion of microplastics by animals in the contexts of food safety and human health risk assessment.
SCOPE
1.1 This practice describes manufacturing methods to create microplastic particles from pellets of common polymers and the preparation of microplastic reference samples for calibration and proficiency evaluation of microplastic collection practices, preparation practices, and identification methods.  
1.2 This practice does not describe methods for controlling or characterizing the shapes of particles. The procedures have been observed to yield irregularly shaped particles, the use of which in many cases will serve to remove the analytical bias inherent with using distinctive manufactured spherical beads. Other procedures should be used if spheres or elongated fibers are desired.  
1.3 This practice does not describe handling procedures for waste generated when executing the procedures described herein. It is the responsibility of the user of this practice to follow applicable laws and regulations when manufacturing and disposing of microplastic particles, and to establish appropriate procedures to minimize the amount of waste generated.  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.5 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 appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.6 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.

General Information

Status
Published
Publication Date
31-Mar-2023
ICS
83.080.01 - Plastics in general
Technical Committee
D19 - Water
Drafting Committee
D19.06 - Methods for Analysis for Organic Substances in Water
Current Stage
Ref Project

Relations

Refers
ASTM D8333-20 - Standard Practice for Preparation of Water Samples with High, Medium, or Low Suspended Solids for Identification and Quantification of Microplastic Particles and Fibers Using Raman Spectroscopy, IR Spectroscopy, or Pyrolysis-GC/MS
Effective Date
15-Jul-2020

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ASTM D8402-23 - Standard Practice for Development of Microplastic Reference Samples for Calibration and Proficiency Evaluation in All Types of Water Matrices with High to Low Levels of Suspended SolidsASTM D8402-23 - Standard Practice for Development of Microplastic Reference Samples for Calibration and Proficiency Evaluation in All Types of Water Matrices with High to Low Levels of Suspended Solids
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ASTM D8402-23 - Standard Practice for Development of Microplastic Reference Samples for Calibration and Proficiency Evaluation in All Types of Water Matrices with High to Low Levels of Suspended Solids
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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: D8402 − 23
Standard Practice for
Development of Microplastic Reference Samples for
Calibration and Proficiency Evaluation in All Types of Water
1
Matrices with High to Low Levels of Suspended Solids
This standard is issued under the fixed designation D8402; 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 2. Referenced Documents
2
2.1 ASTM Standards:
1.1 This practice describes manufacturing methods to create
D883 Terminology Relating to Plastics
microplastic particles from pellets of common polymers and
D1193 Specification for Reagent Water
the preparation of microplastic reference samples for calibra-
D1921 Test Methods for Particle Size (Sieve Analysis) of
tion and proficiency evaluation of microplastic collection
Plastic Materials
practices, preparation practices, and identification methods.
D5905 Practice for the Preparation of Substitute Wastewater
1.2 This practice does not describe methods for controlling
D8333 Practice for Preparation of Water Samples with High,
or characterizing the shapes of particles. The procedures have
Medium, or Low Suspended Solids for Identification and
been observed to yield irregularly shaped particles, the use of
Quantification of Microplastic Particles and Fibers Using
which in many cases will serve to remove the analytical bias
Raman Spectroscopy, IR Spectroscopy, or Pyrolysis-
inherent with using distinctive manufactured spherical beads.
GC/MS
Other procedures should be used if spheres or elongated fibers
3
2.2 ISO Standards:
are desired.
ISO 8573-1:2010 Compressed air — Part 1: Contaminants
1.3 This practice does not describe handling procedures for
and purity classes
waste generated when executing the procedures described
3. Terminology
herein. It is the responsibility of the user of this practice to
3.1 For definitions of terms used in this practice, refer to
follow applicable laws and regulations when manufacturing
Terminology D883.
and disposing of microplastic particles, and to establish appro-
priate procedures to minimize the amount of waste generated.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 glass transition temperature, n—a temperature above
1.4 The values stated in SI units are to be regarded as
which an amorphous material transitions from a relatively
standard. No other units of measurement are included in this
brittle material to a viscous, supercooled liquid.
standard.
3.2.2 microplastic, n—any solid, synthetic organic poly-
1.5 This standard does not purport to address all of the
meric material to which chemical additives or other substances
safety concerns, if any, associated with its use. It is the
may have been added, which are particles <5 mm in their
responsibility of the user of this standard to establish appro-
largest dimension, and fibers no longer than 15 mm in length,
priate safety, health, and environmental practices and deter-
with an aspect ratio of at least 30:1 and <500 μm in its smallest
mine the applicability of regulatory limitations prior to use.
dimension.
1.6 This international standard was developed in accor-
3.2.3 suspended solids, n—includes all matter that is re-
dance with internationally recognized principles on standard-
moved by a 0.45 μm pore size filter.
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
4. Summary of Practice
mendations issued by the World Trade Organization Technical
4.1 Polymer pellets are processed in a laboratory grinder
Barriers to Trade (TBT) Committee.
that utilizes a spinning blade to fragment the pellets into
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
1
This practice is under the jurisdiction of ASTM Committee D19 on Water and contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
is the direct responsibility of Subcommittee D19.06 on Methods for Analysis for Standards volume information, refer to the standard’s Document Summary page on
Organic Substances in Water. the ASTM website.
3
Current edition approved April 1, 2023. Published June 2023. DOI: 10.1520/ Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
D8402-23. 4th Floor, New York, NY 10036, http://www.ansi.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D8402 − 23
powders contain
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ASTM D8333-20(Practice)
Standard Practice for Preparation of Water Samples with High, Medium, or Low Suspended Solids for Identification and Quantification of Microplastic Particles and Fibers Using Raman Spectroscopy, IR Spectroscopy, or Pyrolysis-GC/MS

SIGNIFICANCE AND USE
5.1 Large volumes of water are required to be sieved for accurate quantification of microplastics. Water with high to medium content of suspended solids can lead to an excess of inorganic and organic background material which can interfere with the ability to conduct reliable analyses. The presence of this background material can often impede the ability to accurately discern, distinguish and identify the number of microplastic particles in solution.  
5.2 The digestion described in this procedure allows for significant reduction of interfering substances and contaminants, rendering a sample suitable for particle and fiber characterization and identification using either Raman and IR spectroscopic analysis or for polymeric quantification and identification by Pyrolysis-GC/MS.  
5.3 For water samples with medium to low suspended solids, the oxidation and digestion steps necessary will be dependent upon the type and nature of interfering substances and contaminants and may be determined through simple trial efforts.
SCOPE
1.1 This practice provides for the sample preparation of collected water samples with high, medium, or low suspended solids to determine the presence, count, polymer type, and physical characteristics of microplastic particles and fibers. It has been designed for the preparation of samples collected from drinking water, surface waters, wastewater influent and effluent (secondary and tertiary), and marine waters using collection practice (Practice D8332). This practice is not limited to these particular water matrices; however, the applicability of this practice to other aqueous matrices must be demonstrated.  
1.2 This practice consists of a wet peroxide oxidation followed by progressive enzymatic digestion to the extent necessary to remove interfering organic constituents such as cellulose, lipids and chitin that are typically found in abundance in water matrices of samples with high to medium suspended solids such as wastewater influent. For water samples with low suspended solids, such as but not limited to drinking water and tertiary treated wastewater, the oxidation and digestion steps may not be necessary.  
1.3 Water samples prepared using this practice are suitable for analysis utilizing either Pyrolysis-GC/MS methods for qualitative identification and mass quantitation, or IR spectroscopy or Raman spectroscopy for identifying the quantity (number count) and composition (polymer type) of microplastic particles. If desired, microplastic particle size and shape may be ascertained with appropriate instruments such as a scanning electron microscope (SEM) and microscopy techniques.  
1.4 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.5 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 appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.6 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.

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ASTM D8332-20(Practice)
Standard Practice for Collection of Water Samples with High, Medium, or Low Suspended Solids for Identification and Quantification of Microplastic Particles and Fibers

SIGNIFICANCE AND USE
5.1 When significant quantities of inorganic or organic material are present in water samples (high suspended solids), microplastic particles/fibers can be masked and the ability to conduct reliable identification and quantification analyses of the plastic particles/fibers can be impeded.  
5.2 In order to quantify the occurrence of microplastic particles/fibers in wastewater influent (high suspended solids), the sampling procedure must be able to reliably collect samples at a constant flow over the desired 24-hour interval to reflect changes in diurnal flow. For wastewater influent the capture flow rate should be no less than 1 GPM over the 24-hour interval (approximately 1440 gal or 5450 L total) to minimize the problem with heterogeneity of the suspended solids and to reduce the standard error (the larger the sample size, the smaller the standard error).  
5.3 In order to quantify the occurrence of microplastic particles/fibers in all other water samples with a lower content of inorganic or organic material present addressed by this practice (low to medium suspended solids), a minimum volume of 1500 L (approximately 400 gal) should be filtered through the appropriate filters or sieves to minimize potential issues with heterogeneity of suspended solids and to reduce the standard error (the larger the sample size, the smaller the standard error).  
5.4 Microplastic particles/fibers retained on the sieves are suitable for characterization in terms of size, shape, quantity, and composition (polymer type), dependent upon the chosen analytical method.
SCOPE
1.1 This practice provides for the collection of water samples with high, medium, or low suspended solids to determine the presence, count, polymer type, and physical characteristics of microplastic particles and fibers. This collection practice has been validated for the collection of samples from drinking water, surface waters, wastewater influent and effluent (secondary and tertiary), and marine waters. This practice is not limited to these particular water matrices; however, the applicability of this practice to other aqueous matrices must be demonstrated.  
1.2 Water samples are passed through filters or sieves of adequate mesh size to enable capture of the smallest desired particle size. For waters with high or medium suspended solids content, a series of sieves with increasingly smaller mesh size should be used to prevent clogging and allow for the collection of desired particle size fractions.  
1.3 Subsequent sample preparation followed by analysis utilizing either Pyrolysis gas chromatography/mass spectrometry (Py-GC/MS), IR spectroscopy, or Raman spectroscopy may be used to identify the quantity (mass or number count) and composition (polymer type) of microplastic particles/fibers. The spectroscopic methods can provide a count of the number of particles and fibers present in a sample, and Py-GC/MS can provide the mass present in a sample. When desired, microplastic particle/fiber size, shape and surface characteristics can be ascertained with appropriate instruments such as a scanning electron microscope (SEM).  
1.4 Units—The values stated in SI units are to be regarded as the standard except where standard U.S. equipment is specified in imperial units, for example, inches and gallons. No other units of measurement are included in this standard.  
1.5 Standard Practice—This practice offers a set of instructions for performing one or more specific operations. This practice cannot replace education or experience and should be used in conjunction with professional judgment. Not all aspects of this practice may be applicable in all circumstances. This practice is not intended to represent or replace the standard of care by which the adequacy of a given professional service must be judged, nor should this practice be applied without consideration of a project’s many unique aspects.  
1.6 This standard does not purport to addre...

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ASTM E2113-23(Test Method)
Standard Test Method for Length Change Calibration of Thermomechanical Analyzers

SIGNIFICANCE AND USE
5.1 Performance verification or calibration is essential to the accurate determination of quantitative dimension change measurements.  
5.2 This test method may be used for instrument performance validation, regulatory compliance, research and development and quality assurance purposes.
SCOPE
1.1 This test method describes calibration of the length change (deflection) measurement or thermal expansion of thermomechanical analyzers (TMAs) within the temperature range from –150 °C to 1000 °C using the thermal expansion of a suitable reference material.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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ASTM D695-23(Test Method)
Standard Test Method for Compressive Properties of Rigid Plastics

SIGNIFICANCE AND USE
4.1 Compression tests provide information about the compressive properties of plastics when employed under conditions approximating those under which the tests are made.  
4.2 Compressive properties include modulus of elasticity, yield stress, deformation beyond yield point, and compressive strength (unless the material merely flattens but does not fracture). Materials possessing a low order of ductility may not exhibit a yield point. In the case of a material that fails in compression by a shattering fracture, the compressive strength has a very definite value. In the case of a material that does not fail in compression by a shattering fracture, the compressive strength is an arbitrary one depending upon the degree of distortion that is regarded as indicating complete failure of the material. Many plastic materials will continue to deform in compression until a flat disk is produced, the compressive stress (nominal) rising steadily in the process, without any well-defined fracture occurring. Compressive strength can have no real meaning in such cases.  
4.3 Compression tests provide a standard method of obtaining data for research and development, quality control, acceptance or rejection under specifications, and special purposes. The tests cannot be considered significant for engineering design in applications differing widely from the load-time scale of the standard test. Such applications require additional tests such as impact, creep, and fatigue.  
4.4 Before proceeding with this test method, reference should be made to the ASTM specification for the material being tested. Any test specimen preparation, conditioning, dimensions, and testing parameters covered in the materials specification shall take precedence over those mentioned in this test method. If there is no material specification, then the default conditions apply. Table 1 in Classification D4000 lists the ASTM materials standards that currently exist.
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1.2 The values stated in SI units are to be regarded as the standard. The values in parentheses are for information only.
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4.1 Tests made under conditions herein prescribed can be of considerable value in comparing the relative ignition characteristics of different materials. Values obtained represent the lowest ambient air temperature that will cause ignition of the material under the conditions of this test. Test values are expected to rank materials according to ignition susceptibility under actual use conditions.  
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1.1 This fire test response test method2 covers a laboratory determination of the flash ignition temperature and spontaneous ignition temperature of plastics using a hot-air furnace.  
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1.4 This standard is used to measure and describe the response of materials, products, or assemblies to heat and flame under controlled conditions, but does not by itself incorporate all factors required for fire-hazard or fire-risk assessment of the materials, products, or assemblies under actual fire conditions.  
1.5 Fire testing is inherently hazardous. Adequate safeguards for personnel and property shall be employed in conducting these tests.  
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 appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific precautionary statements are given in 1.3 and 1.4.
Note 1: This test method and ISO 871-2022 (Option 1) are similar in all technical details.  
1.7 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.

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ASTM D3929-03(2023)(Test Method)
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SIGNIFICANCE AND USE
5.1 This test method is designed for obtaining a qualitative estimate of the compatibility of plastics and adhesives. Due to the many process variables associated with the fabrication of plastic parts, it is not possible to use this test as a substitute for compatibility tests on actual parts.  
5.2 The detection of cracks or crazes may be determined with or without optical aid. Make comparisons only among tests employing crack detection methods of equivalent sensitivity.
SCOPE
1.1 This test method describes a procedure for determining the compatibility of adhesives with plastics based on whether the adhesive causes cracking of stressed samples.  
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SIGNIFICANCE AND USE
4.1 The purpose of this classification system is to provide a method of adequately identifying plastic materials in order to give industry a system that can be used universally for plastic materials. It further provides a means for specifying these materials by the use of a simple line call-out designation.  
4.2 This classification system was developed to permit the addition of property values for future plastics.
SCOPE
1.1 This standard provides a classification system for tabulating the properties of unfilled, filled, and reinforced plastic materials suitable for processing into parts.
Note 1: The classification system serves many of the needs of industries using plastic materials. The standard is subject to revision as the need requires; therefore, the latest revision should always be used.  
1.2 The classification system and subsequent line call-out (specification) is intended to be a means of identifying plastic materials used in the fabrication of end items or parts. It is not intended for the selection of materials. Material selection should be made by those having expertise in the plastics field after careful consideration of the design and the performance required of the part, the environment to which it will be exposed, the fabrication process to be employed, the inherent properties of the material not covered in this document, and the economic factors.  
1.3 This classification system is based on the premise that plastic materials can be arranged into broad generic families using basic properties to arrange the materials into groups, classes, and grades. A system is thus established which, together with values describing additional requirements, permits as complete a description as desired of the selected material.  
1.4 In all cases where the provisions of this classification system would conflict with the referenced ASTM specification for a particular material, the latter shall take precedence.  
Note 2: When using this classification system the two-letter, three-digit suffix system applies.
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ASTM F640-23(Test Method)
Standard Test Methods for Determining Radiopacity for Medical Use

SIGNIFICANCE AND USE
5.1 These methods are intended to determine whether a material, product, or part of a product has the degree of radiopacity desired for its application as a medical device in the human body. This method allows for comparison with or without the use of a body mimic. Comparisons without the use of a body mimic should be used with caution as the relative radiopacity can be affected when imaging through the human body.  
5.2 These methods allow for both qualitative and quantitative evaluation in different comparative situations.
SCOPE
1.1 These test methods cover the determination of the radiopacity of materials and products utilizing X-ray based techniques, including fluoroscopy, angiography, CT (computed tomography), and DEXA (dual energy X-ray absorptiometry), also known as DXA, The results of these measurements are an indication of the likelihood of locating the product within the human body.  
1.2 Radiopacity is determined by (a) qualitatively comparing image(s) of a test specimen and a user-defined standard, with or without the use of a body mimic; or (b) quantitatively determining the specific difference in optical density or pixel intensity between the image of a test specimen and the image of a user-defined standard, with or without the use of a body mimic.  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 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 appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 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.

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Standard Guide for Description of Polymer Pellet Defects

SIGNIFICANCE AND USE
4.1 This guide is intended to provide terminology for both suppliers and users of polymer pellets to ensure mutual understanding in discussions concerning pellet defects. It is not an absolute standard but is to be referred to when issues with the quality and/or description of the polymeric materials arise.  
4.2 The guide is categorized according to the best fit for the term and its description for ease of finding certain description types.  
4.3 Some terms within this guide do not apply to all resin types. It is the user’s responsibility to determine if the term and its subsequent definition are applicable to the material in question.  
4.4 Other terminology relating to polymers that are not included in this document can be found in additional standards such as Terminology D883.  
4.5 Test Method D6290 can be used for the instrumental measurement of discoloration in plastics, including pellets, and of the degree of yellowness (or change of degree of yellowness) under daylight illumination of homogeneous, nonfluorescent, nearly colorless transparent or nearly-white translucent or opaque plastics.
SCOPE
1.1 This guide is a compilation of terms used to describe defects of polymeric pellets. Terms that are generally understood or defined adequately in readily available sources are not included.  
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1.3 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 appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
Note 1: There is no known ISO equivalent to this guide.  
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ASTM G22-23(Practice)
Standard Practice for Determining Resistance of Plastics to Bacteria

SIGNIFICANCE AND USE
4.1 The resin portion of plastic materials is usually resistant to bacteria, in that it does not serve as a carbon source for the growth of bacteria. It is generally the other components, such as plasticizers, lubricants, stabilizers, and colorants that are responsible for bacterial attack on plastic materials. It is important to establish the resistance of plastics to microbial attack when plastics are used under conditions of high temperature and humidity favorable for such attack.  
4.2 The effects to be expected are:  
4.2.1 Surface attack, discoloration, and loss of transmission (optical).  
4.2.2 Removal of susceptible plasticizers, modifiers, and lubricants, resulting in increased modulus (stiffness), changes in weight, dimensions, and other physical properties, and deterioration of electrical properties such as insulation resistance, dielectric constant, power factor, and dielectric strength.  
4.3 Often the changes in electrical properties are due principally to surface growth and associated moisture, and to pH changes caused by products of bacterial metabolism. Other effects include preferential growths caused by nonuniform dispersion of plasticizers, lubricants, and other processing additives. Pronounced physical changes may be observed on products in film form or as coatings where the ratio of surface to volume is high, and where nutrient materials such as plasticizers and lubricants continue to diffuse to the surface as they are utilized by the organisms.  
4.4 Since attack by organisms involves a large element of change due to local accelerations and inhibitions, the order of reproducibility may be rather low. To assure that estimates of behavior are not too optimistic, the greatest observed degree of deterioration should be reported.  
4.5 Conditioning of specimens such as exposure to leaching, weathering, heat treatment, etc., may have significant effects on the resistance of plastics to bacteria. Determination of these effects is not covered i...
SCOPE
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1.2 The values stated in SI units are to be regarded as the standard.  
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