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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Publication Date
14-Jul-2020
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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
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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: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
1
Spectroscopy, IR Spectroscopy, or Pyrolysis-GC/MS
This standard is issued under the fixed designation D8333; 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 1.5 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
1.1 This practice provides for the sample preparation of
responsibility of the user of this standard to establish appro-
collected water samples with high, medium, or low suspended
priate safety, health, and environmental practices and deter-
solids to determine the presence, count, polymer type, and
mine the applicability of regulatory limitations prior to use.
physical characteristics of microplastic particles and fibers. It
1.6 This international standard was developed in accor-
has been designed for the preparation of samples collected
dance with internationally recognized principles on standard-
from drinking water, surface waters, wastewater influent and
ization established in the Decision on Principles for the
effluent (secondary and tertiary), and marine waters using
Development of International Standards, Guides and Recom-
collection practice (Practice D8332). This practice is not
mendations issued by the World Trade Organization Technical
limited to these particular water matrices; however, the appli-
Barriers to Trade (TBT) Committee.
cability of this practice to other aqueous matrices must be
demonstrated.
2. Referenced Documents
1.2 This practice consists of a wet peroxide oxidation 2
2.1 ASTM Standards:
followed by progressive enzymatic digestion to the extent
D883 Terminology Relating to Plastics
necessary to remove interfering organic constituents such as
D1193 Specification for Reagent Water
cellulose, lipids and chitin that are typically found in abun-
D8332 Practice for Collection of Water Samples with High,
dance in water matrices of samples with high to medium
Medium, or Low Suspended Solids for Identification and
suspended solids such as wastewater influent. For water
Quantification of Microplastic Particles and Fibers
samples with low suspended solids, such as but not limited to
drinking water and tertiary treated wastewater, the oxidation
3. Terminology
and digestion steps may not be necessary.
3.1 Definitions:
1.3 Water samples prepared using this practice are suitable
3.1.1 For definitions of terms used in this standard, refer to
for analysis utilizing either Pyrolysis-GC/MS methods for
Terminology D883.
qualitative identification and mass quantitation, or IR spectros-
3.2 Definitions of Terms Specific to This Standard:
copy or Raman spectroscopy for identifying the quantity
3.2.1 effluent, n—any stage of treated wastewater.
(number count) and composition (polymer type) of microplas-
3.2.2 influent, n—raw sewage entering a wastewater treat-
tic particles. If desired, microplastic particle size and shape
ment facility.
may be ascertained with appropriate instruments such as a
scanning electron microscope (SEM) and microscopy tech-
3.2.3 microplastic, n—any solid, synthetic organic poly-
niques.
meric material to which chemical additives or other substances
may have been added, which are particles <5 mm in their
1.4 Units—The values stated in SI units are to be regarded
largest dimension, and fibers no longer than 15 mm in length
as standard. No other units of measurement are included in this
with an aspect ratio of at least 30:1 and <500 µm in its smallest
standard.
dimension.
1
This practice is under the jurisdiction of ASTM Committee D19 on Water and
2
is the direct responsibility of Subcommittee D19.06 on Methods for Analysis for For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Organic Substances in Water. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Current edition approved July 15, 2020. Published August 2020. DOI: 10.1520/ Standards volume information, refer to the standard’s Document Summary page on
D8333-20. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D8333−20
3.2.4 surface waters, n—a water body with its surface in 6. Reagents and Materials
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