ASTM D4489-95(2024)

Standard Practices for Sampling of Waterborne Oils

SIGNIFICANCE AND USE
4.1 Identification of the source of a spilled oil is established by comparison with known oils selected because of their possible relationship to the spill, that is, potential sources. Generally, the suspected source oils are from pipelines, tanks, etc., and therefore pose little problems in sampling compared to the spilled oil. This practice addresses the sampling of spilled oils in particular, but could be applied to appropriate source situations, for example, a ship's bilge.
SCOPE
1.1 These practices describe the procedures to be used in collecting samples of waterborne oils (see Practice D3415), oil found on adjoining shorelines, or oil-soaked debris, for comparison of oils by spectroscopic and chromatographic techniques, and for elemental analyses.  
1.2 Two practices are described. Practice A involves “grab sampling” macro oil samples. Practice B can be used to sample most types of waterborne oils and is particularly applicable in sampling thin oil films or slicks. Practice selection will be dictated by the physical characteristics and the location of the spilled oil. These two practices are:    
Sections  
Practice A (for grab sampling thick layers of oil, viscous oils or oil soaked debris, oil globules, tar balls, or stranded oil)  
9 to 13  
Practice B (for TFE–fluorocarbon polymer strip samplers)  
14 to 17  
1.3 Each of the two practices is designed to collect oil samples with a minimum of water, thereby reducing the possibility of chemical, physical, or biological alteration by prolonged contact with water between the time of collection and analysis.  
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. For specific hazards statements, see Section 7.  
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-2024
• ICS: 75.040 - Crude petroleum
• Technical Committee: D19 - Water
• Drafting Committee: D19.06 - Methods for Analysis for Organic Substances in Water

Relations

• Replaces: ASTM D4489-95(2017) - Standard Practices for Sampling of Waterborne Oils
• Effective Date: 01-Apr-2024
• Refers: ASTM D3415-98(2024) - Standard Practice for Identification of Waterborne Oils
• Effective Date: 01-Apr-2024
• Refers: ASTM D3415-98(2017) - Standard Practice for Identification of Waterborne Oils
• Effective Date: 15-Dec-2017
• Referred By: ASTM D5412-93(2017)e1 - Standard Test Method for Quantification of Complex Polycyclic Aromatic Hydrocarbon Mixtures or Petroleum Oils in Water
• Effective Date: 01-Apr-2024
• Referred By: ASTM D3325-90(2020) - Standard Practice for Preservation of Waterborne Oil Samples
• Effective Date: 01-Apr-2024
• Referred By: ASTM D3326-07(2024) - Standard Practice for Preparation of Samples for Identification of Waterborne Oils
• Effective Date: 01-Apr-2024
• Referred By: ASTM D3328-06(2020) - Standard Test Methods for Comparison of Waterborne Petroleum Oils by Gas Chromatography
• Effective Date: 01-Apr-2024
• Referred By: ASTM E2143-01(2021) - Standard Test Method for Using Field-Portable Fiber Optics Synchronous Fluorescence Spectrometer for Quantification of Field Samples for Aromatic and Polycyclic Aromatic Hydrocarbons
• Effective Date: 01-Apr-2024

Overview

ASTM D4489-95(2024): Standard Practices for Sampling of Waterborne Oils is an internationally recognized standard developed by ASTM International. This standard outlines best practices and practical techniques for the collection of samples of waterborne oils-including oil on adjoining shorelines and oil-soaked debris-for the analysis and identification of possible sources of spilled oil. Through careful application of these procedures, it ensures collected samples remain representative and uncontaminated, enabling accurate comparison using spectroscopic, chromatographic, and elemental analysis.

The standard is frequently applied in environmental monitoring, marine spill response, and forensic investigations relating to petroleum and oil-based contaminants.

Key Topics

• Sampling Objectives: Ensures the collection of representative oil samples with minimal water content to avoid physical, chemical, or biological changes before analysis.
• Two Main Practices:
  • Practice A: Grab sampling for thick oil layers, viscous oils, oil-globules, tar balls, stranded oil on shorelines, or oil-soaked debris.
  • Practice B: Use of TFE-fluorocarbon polymer strip or mesh samplers, highly effective for thin films or oil slicks on water surfaces.
• Chain of Custody: Emphasizes documented accountability for samples to ensure integrity and defend the results of oil identification analyses.
• Sample Container and Handling: Utilizes cleaned glass jars with TFE-fluorocarbon or aluminum-coated lids; use of high-purity solvents for container rinsing is specified.
• Labeling and Documentation: Mandatory detailed labeling (sample ID, date, location, collector signatures, and witness) to maintain traceability.
• Health & Safety Practices: Highlights the importance of minimizing risks during sampling, especially relating to solvent use and contact with crude oil.
• Sample Storage: Recommends refrigeration at 4°C to 5°C to prevent sample degradation during storage and transportation.

Applications

• Oil Spill Response: Guides emergency and field responders in collecting oil samples from spills on water, shorelines, or contaminated debris for subsequent laboratory analysis.
• Environmental Forensics: Enables comparison of spilled oils with potential source oils (from pipelines, ships, storage tanks) to support pollution tracing, liability enforcement, and remediation.
• Regulatory Compliance: Assists organizations in meeting legal and regulatory requirements for oil spill monitoring and documentation, particularly when handling waterborne petroleum pollutants.
• Research & Monitoring: Used by scientists and environmental agencies to systematically monitor petroleum contamination in aquatic environments.

Key benefits include:

• Improved reliability and accuracy in oil spill identification
• Minimization of contamination and alteration of samples
• Standardized approach supporting international regulatory and legal frameworks

Related Standards

The following standards are referenced or related to ASTM D4489-95(2024):

• ASTM D1129: Terminology Relating to Water - provides fundamental definitions used in sampling and analysis.
• ASTM D3415: Practice for Identification of Waterborne Oils - complements D4489 procedures with identification methodologies.
• World Trade Organization (WTO) TBT Principles: Ensures alignment with internationally recognized principles for standardization under the Technical Barriers to Trade Committee.

By following ASTM D4489-95(2024), organizations can ensure consistent, reliable, and defensible sampling of waterborne petroleum oils, critical for effective environmental management and incident response. For more information, visit the ASTM International website or consult the Annual Book of ASTM Standards.

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: D4489 − 95 (Reapproved 2024)
Standard Practices for
Sampling of Waterborne Oils
This standard is issued under the fixed designation D4489; 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
1.1 These practices describe the procedures to be used in 2.1 ASTM Standards:
collecting samples of waterborne oils (see Practice D3415), oil D1129 Terminology Relating to Water
D3415 Practice for Identification of Waterborne Oils
found on adjoining shorelines, or oil-soaked debris, for com-
parison of oils by spectroscopic and chromatographic
3. Terminology
techniques, and for elemental analyses.
3.1 Definitions:
1.2 Two practices are described. Practice A involves “grab
3.1.1 For definitions of terms used in this standard, refer to
sampling” macro oil samples. Practice B can be used to sample
Terminology D1129.
most types of waterborne oils and is particularly applicable in
sampling thin oil films or slicks. Practice selection will be
3.2 Definitions of Terms Specific to This Standard:
dictated by the physical characteristics and the location of the
3.2.1 chain of custody, n—a documented accountability of
spilled oil. These two practices are:
each sample, that is, date, time, and signature of each recipient
Sections when the sample changes hands, from the time of collection
Practice A (for grab sampling thick layers of oil, viscous oils or 9 to 13
until the requirement for each sample is terminated.
oil soaked debris, oil globules, tar balls, or stranded oil)
Practice B (for TFE–fluorocarbon polymer strip samplers) 14 to 17 3.2.2 waterborne oil, n—refer to Practice D3415.
1.3 Each of the two practices is designed to collect oil
4. Significance and Use
samples with a minimum of water, thereby reducing the
4.1 Identification of the source of a spilled oil is established
possibility of chemical, physical, or biological alteration by
prolonged contact with water between the time of collection by comparison with known oils selected because of their
possible relationship to the spill, that is, potential sources.
and analysis.
Generally, the suspected source oils are from pipelines, tanks,
1.4 The values stated in SI units are to be regarded as
etc., and therefore pose little problems in sampling compared
standard. No other units of measurement are included in this
to the spilled oil. This practice addresses the sampling of
standard.
spilled oils in particular, but could be applied to appropriate
1.5 This standard does not purport to address all of the
source situations, for example, a ship’s bilge.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
5. Apparatus
priate safety, health, and environmental practices and deter-
5.1 Sample Containers, 100 mL to 125 mL wide-mouth
mine the applicability of regulatory limitations prior to use.
glass jars that have been thoroughly cleaned. When field
For specific hazards statements, see Section 7.
expedients must be employed, an empty container of each type
1.6 This international standard was developed in accor-
used should be included in the shipment to the laboratory, to be
dance with internationally recognized principles on standard-
used as a blank to measure inadvertent contamination.
ization established in the Decision on Principles for the
5.2 Closures—Lids for the glass jars should have TFE-
Development of International Standards, Guides and Recom-
fluorocarbon polymer film or aluminum-coated insert.
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
5.3 Strip Samplers, 5 cm by 7.5 cm pieces of TFE-
fluorocarbon polymer sheets (0.25 mm thickness, or screen or
fabric (50–70 mesh)).
These practices are under the jurisdiction of ASTM Committee D19 on Water
and are the direct responsibility of Subcommittee D19.06 on Methods for Analysis
for Organic Substances in Water. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved April 1, 2024. Published April 2024. Originally contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
approved in 1985. Last previous edition approved in 2017 as D4489 – 95 (2017). Standards volume information, refer to the standard’s Document Summary page on
DOI: 10.1520/D4489-95R24. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4489 − 95 (2024)
NOTE 1—Storage at lower temperatures (−10 °C or lower) may cause
5.4 Wooden Tongue Depressor.
irreversible crystallization of waxes. Storage at 4 °C to 5 °C obviates this
5.5 TFE-Fluorocarbon Polymer Net Sampling Kit.
problem; biological degradation at 4 °C to 5 °C has been found negligible
over a 3 to 5-year storage with respect to qualitative identification of oil.
6. Reagents
PRACTICE A—GRAB SAMPLING
6.1 High Purity Solvents, that must be used for rinsing
samplers and sample containers. The solvents which may be
9. Scope
used are n-hexane, mixed hexanes, cyclohexane, pentane, or
9.1 This practice is applicable to thick layers of waterborne
dichloromethane, acetone, or chloroform.
oil films, viscous oils, oil globules, and tar balls.
7. Hazards
9.2 This practice is also applicable to sampling oil stranded
on shorelines or oil-soaked debris.
7.1 Precaution—Extreme care should be exercised so as
not to contaminate the samples or cause their integrity to be
questioned. 10. Summary of Practice
10.1 The sampling consists of collecting the sample directly
7.2 Warning—The rinsing solvents are volatile and, except
for dichloromethane, are flammable, and therefore should be with the sample container, that is, scooping the sample up in
the sample jar and sealing.
handled with appropriate care. Dichloromethane will release
toxic vapors when heated.
11. Apparatus
7.3 Minimize contact with oil even when wearing gloves.
11.1 The sample container serves as the sampling device
8. General Sampling Guidelines
(see 5.1). The glass jars and lid liners should be rinsed three
times with a high purity solvent (see 6.1), allowed to air dry,
8.1 The objective is to obtain a sample for analysis that is
and assembled prior to use. Sample jars that are precleaned
representative of the spilled oil. The most critical factors in
using EPA-recommended wash procedures for organics are
sampling are selecting a suitable location, collecting a sample
acceptable.
of oil with the least water possible (to minimize possible
sample alteration), and maintaining the sample integrity.
NOTE 2—To avoid possible sample contamination, do not reuse sample
containers, lids, or liners.
8.2 It is recommended that at least three samples be taken of
11.2 Nitrile gloves are to be worn during sampling.
each waterborne oil in order to demonstrate the homogeneity of
the spill. These samples should be taken in different regions of
11.3 A detachable ring for the sample jar and sampling pole
the oil slick at points where the accumulation is heaviest. This
may be useful to extend sampling range.
will increase the volume of oil available for analysis. In the
event that multiple samples cannot be collected, then a single
12. Procedure for Floating Samples
sample should be collected from the area where the accumu-
12.1 Select the sampling site.
lation of oil visually appears to be the heaviest.
12.2 Unscrew the lid from the sample jar. Hold the jar in
8.3 The following general rules are applicable to sampling
position for sampling; hold the lid in a free hand or place the
of waterborne oils:
lid in a safe position. Gently lower the sample jar into the water
8.3.1 Take a sample that contains sufficient oil for the
and gently skim the oil layer or oil globules from the water
method or methods of analysis to be employed and for any
surface into the sample container. Continue the process until
replicate analyses that may be required.
the sample container is approximately three-quarters full.
8.3.2 Affix a label or tag to the sample jar in such a manner
that it becomes an integral part of the container. The label or 12.3 Remove the sample container from the water surface,
tag should contai
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