ASTM D3650-93(2011)
(Test Method)Standard Test Method for Comparison of Waterborne Petroleum Oils By Fluorescence Analysis (Withdrawn 2018)
Standard Test Method for Comparison of Waterborne Petroleum Oils By Fluorescence Analysis (Withdrawn 2018)
SIGNIFICANCE AND USE
This test method is useful for rapid identification of waterborne petroleum oil samples as well as oil samples obtained from fuel or storage tanks, or from sand, vegetation, or other substrates. This test method is applicable to weathered and unweathered neat oil samples.
The unknown oil is identified through the comparison of the fluorescence spectrum of the oil with the spectra (obtained at similar instrumental settings on the same instrument) of possible source samples. A match of the entire spectrum between the unknown and possible source sample indicates a common source.
SCOPE
1.1 This test method covers the comparison of waterborne petroleum oils with oils from possible sources by means of fluorescence spectroscopy (1). Useful references for this test method include: (2) and (3) for fluorescence analysis in general and (4), (5), and (6) for oil spill identification including fluorescence.
1.2 This test method is applicable to crude or refined petroleum products, for any sample of neat oil, waterborne oil, or sample of oil-soaked material. Unless the samples are collected soon after the spill occurs, it is not recommended that volatile fuels such as gasoline, kerosine, and No. 1 fuel oils be analyzed by this test method, because their fluorescence signatures change rapidly with weathering. Some No. 2 fuel oils and light crude oils may only be identifiable up to 2 days weathering, or less, depending on the severity of weathering. In general, samples weathered up to 1 week may be identified, although longer periods of weathering may be tolerated for heavy residual oils, oil weathered under Arctic conditions, or oil that has been protected from weathering by collecting in a thick layer.
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 and health practices and determine the applicability of regulatory limitations prior to use.
WITHDRAWN RATIONALE
This test method covers the comparison of waterborne petroleum oils with oils from possible sources by means of fluorescence spectroscopy.
Formerly under the jurisdiction of Committee D19 on Water, this test method was withdrawn in November 2018. This standard was withdrawn without replacement due to its limited use by the industry.
General Information
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:D3650 −93 (Reapproved 2011)
Standard Test Method for
Comparison of Waterborne Petroleum Oils By
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Fluorescence Analysis
This standard is issued under the fixed designation D3650; 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
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2.1 ASTM Standards:
1.1 This test method covers the comparison of waterborne
D1129 Terminology Relating to Water
petroleum oils with oils from possible sources by means of
2
D1193 Specification for Reagent Water
fluorescence spectroscopy (1). Useful references for this test
D3325 Practice for Preservation of Waterborne Oil Samples
methodinclude: (2)and (3)forfluorescenceanalysisingeneral
D3326 Practice for Preparation of Samples for Identification
and (4), (5), and (6) for oil spill identification including
of Waterborne Oils
fluorescence.
D3415 Practice for Identification of Waterborne Oils
1.2 This test method is applicable to crude or refined
D4489 Practices for Sampling of Waterborne Oils
petroleum products, for any sample of neat oil, waterborne oil,
E131 Terminology Relating to Molecular Spectroscopy
or sample of oil-soaked material. Unless the samples are
E275 Practice for Describing and Measuring Performance of
collectedsoonafterthespilloccurs,itisnotrecommendedthat
Ultraviolet and Visible Spectrophotometers
volatile fuels such as gasoline, kerosine, and No. 1 fuel oils be
E520 Practice for Describing Photomultiplier Detectors in
analyzed by this test method, because their fluorescence
Emission and Absorption Spectrometry
signatures change rapidly with weathering. Some No. 2 fuel
oils and light crude oils may only be identifiable up to 2 days
3. Terminology
weathering,orless,dependingontheseverityofweathering.In
3.1 Definitions—For definitions of terms used in this test
general, samples weathered up to 1 week may be identified,
method refer to Terminology D1129, Practice D3415, and
although longer periods of weathering may be tolerated for
Terminology E131.
heavy residual oils, oil weathered under Arctic conditions, or
4. Summary of Test Method
oil that has been protected from weathering by collecting in a
thick layer.
4.1 This test method consists of fluorescence analyses of
dilute solutions of oil in spectroquality cyclohexane. In most
1.3 The values stated in SI units are to be regarded as
cases the emission spectra, with excitation at 254 nm, over the
standard. No other units of measurement are included in this
spectral range from 280 to 500 nm, are adequate for matching.
standard.
4.2 Identification of the sample is made by direct visual
1.4 This standard does not purport to address all of the
comparison of the sample’s spectrum with the spectra from
safety concerns, if any, associated with its use. It is the
possible source samples.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
NOTE 1—When weathering has occurred, it may be necessary to
bility of regulatory limitations prior to use. consider known weathering trends when matching spectra (Fig. 1 and Fig.
2).
5. Significance and Use
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This test method is under the jurisdiction of ASTM Committee D19 on Water
5.1 This test method is useful for rapid identification of
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor
waterborne petroleum oil samples as well as oil samples
Organic Substances in Water.
Current edition approved May 1, 2011. Published June 2011. Originally
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approved in 1978. Last previous edition approved in 2006 as D3650 – 93 (2006). For referenced ASTM standards, visit the ASTM website, www.astm.org, or
DOI: 10.1520/D3650-93R11. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
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The boldface numbers in parentheses refer to the references at the end of this Standards volume information, refer to the standard’s Document Summary page on
test method. the ASTM website.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D3650−93 (2011)
6.3 Possible interferences from Raman or RayleighTyndall
scattering are not observed in the emission scan ranges
selected.
7. Apparatus
7.1 Fluorescence Spectrophotometer (or Spectro-
fluorometer)—An instrument recording in the spectral range of
220 nm to at least 600 nm for both excitation and emission
responses and capable of meeting the specifications stated in
Table 1.
7.2 Excitation Source—A high-pressure xenon lamp (a
150-W xeno
...
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