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ASTM D3328-06(2020)

(Test Method)

Standard Test Methods for Comparison of Waterborne Petroleum Oils by Gas Chromatography

Standard Test Methods for Comparison of Waterborne Petroleum Oils by Gas Chromatography

SIGNIFICANCE AND USE
4.1 Identification of a recovered oil is determined by comparison with known oils, selected because of their possible relationship to the particular recovered oil. The known oils are collected from suspected sources. Samples of such known oils must be collected and submitted along with the unknown for analysis. At present, identification of the source of an unknown oil by itself cannot be made (for example, from a library of known oils).  
4.2 The use of a flame-photometric detector in addition to the flame-ionization detector provides a second, independent profile of the same oil, that is, significantly more information is available from a single analysis with dual detection.  
4.3 Many close similarities (within uncertainties of sampling and analysis) will be needed to establish identity beyond a reasonable doubt. The analyses described will distinguish many, but not all samples. For cases in which this method does not clearly identify a pair of samples, and for important cases where additional comparisons are needed to strengthen conclusions, other analyses will be required (refer to Practice D3415). In particular, Practice D5739 is useful for such cases.
SCOPE
1.1 This test method covers the comparison of petroleum oils recovered from water or beaches with oils from suspect sources by means of gas chromatography (1-3).2 Such oils include distillate fuel, lubricating oil, and crude oil. The test method described is for capillary column analyses using either single detection (flame ionization) or dual detection (flame ionization and flame photometric) for sulfur containing species.  
1.2 This test method provides high resolution for critical examination of fine structure that is resistant to weathering. The flame-photometric detection for sulfur components is an adjunct, not a substitute, for flame-ionization detection in the identification of waterborne petroleum oils (4-12). For this reason, flame photometric detection is optional.  
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.

General Information

Status
Published
Publication Date
31-Dec-2019
ICS
75.080 - Petroleum products 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 D4489-95(2017) - Standard Practices for Sampling of Waterborne Oils
Effective Date
15-Dec-2017
Refers
ASTM D3326-07(2017) - Standard Practice for Preparation of Samples for Identification of Waterborne Oils
Effective Date
15-Dec-2017
Refers
ASTM D3415-98(2017) - Standard Practice for Identification of Waterborne Oils
Effective Date
15-Dec-2017
Referred By
ASTM D5739-06(2020) - Standard Practice for Oil Spill Source Identification by Gas Chromatography and Positive Ion Electron Impact Low Resolution Mass Spectrometry
Effective Date
01-Jan-2020
Referred By
ASTM D3325-90(2020) - Standard Practice for Preservation of Waterborne Oil Samples
Effective Date
01-Jan-2020
Referred By
ASTM D8506-23 - Standard Guide for Microbial Contamination and Biodeterioration in Turbine Oils and Turbine Oil Systems
Effective Date
01-Jan-2020
Referred By
ASTM D6469-20 - Standard Guide for Microbial Contamination in Fuels and Fuel Systems
Effective Date
01-Jan-2020
Referred By
ASTM E3361-22 - Standard Guide for Estimating Natural Attenuation Rates for Non-Aqueous Phase Liquids in the Subsurface
Effective Date
01-Jan-2020

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ASTM D3328-06(2020) - Standard Test Methods for Comparison of Waterborne Petroleum Oils by Gas ChromatographyASTM D3328-06(2020) - Standard Test Methods for Comparison of Waterborne Petroleum Oils by Gas Chromatography
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ASTM D3328-06(2020) - Standard Test Methods for Comparison of Waterborne Petroleum Oils by Gas Chromatography
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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: D3328 − 06 (Reapproved 2020)
Standard Test Methods for
Comparison of Waterborne Petroleum Oils by Gas
1
Chromatography
This standard is issued under the fixed designation D3328; 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
3
1.1 This test method covers the comparison of petroleum 2.1 ASTM Standards:
oils recovered from water or beaches with oils from suspect D1129 Terminology Relating to Water
2
sources by means of gas chromatography (1-3). Such oils D1193 Specification for Reagent Water
include distillate fuel, lubricating oil, and crude oil. The test D2549 Test Method for Separation of Representative Aro-
method described is for capillary column analyses using either matics and Nonaromatics Fractions of High-Boiling Oils
single detection (flame ionization) or dual detection (flame by Elution Chromatography
ionization and flame photometric) for sulfur containing spe- D3325 Practice for Preservation of Waterborne Oil Samples
cies. D3326 Practice for Preparation of Samples for Identification
of Waterborne Oils
1.2 This test method provides high resolution for critical
D3415 Practice for Identification of Waterborne Oils
examination of fine structure that is resistant to weathering.
D4489 Practices for Sampling of Waterborne Oils
The flame-photometric detection for sulfur components is an
D5739 Practice for Oil Spill Source Identification by Gas
adjunct, not a substitute, for flame-ionization detection in the
Chromatography and Positive Ion Electron Impact Low
identification of waterborne petroleum oils (4-12). For this
Resolution Mass Spectrometry
reason, flame photometric detection is optional.
E355 Practice for Gas ChromatographyTerms and Relation-
1.3 The values stated in SI units are to be regarded as
ships
standard. No other units of measurement are included in this
3. Terminology
standard.
1.4 This standard does not purport to address all of the
3.1 Definitions:
safety concerns, if any, associated with its use. It is the 3.1.1 For definitions of terms used in this standard, refer to
responsibility of the user of this standard to establish appro-
Practice D3415, Terminology D1129, and Practice E355.
priate safety, health, and environmental practices and deter-
4. Significance and Use
mine the applicability of regulatory limitations prior to use.
4.1 Identification of a recovered oil is determined by com-
1.5 This international standard was developed in accor-
dance with internationally recognized principles on standard- parison with known oils, selected because of their possible
relationship to the particular recovered oil. The known oils are
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom- collected from suspected sources. Samples of such known oils
must be collected and submitted along with the unknown for
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee. analysis.At present, identification of the source of an unknown
oil by itself cannot be made (for example, from a library of
known oils).
1
4.2 The use of a flame-photometric detector in addition to
These test methods are under the jurisdiction of ASTM Committee D19 on
Waterand are the direct responsibility of Subcommittee D19.06 on Methods for
the flame-ionization detector provides a second, independent
Analysis for Organic Substances in Water.
Current edition approved Jan. 1, 2020. Published January 2020. Originally
3
approved in 1974. Last previous edition approved in 2013 as D3328 – 06 (2013). For referenced ASTM standards, visit the ASTM website, www.astm.org, or
DOI: 10.1520/D3328-06R20. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
2
The boldface numbers in parentheses refer to a list of references at the end of Standards volume information, refer to the standard’s Document Summary page on
this standard. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D3328 − 06 (2020)
profileofthesameoil,thatis,significantlymoreinformationis 7. Reference Standards
available from a single analysis with dual detection.
7.1 Normal Paraffınic Hydrocarbons—Prepared mixtures of
4.3 Many close similarities (within uncertainties of sam-
approximately decane to hexatriacontane, or selected indi-
...

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ASTM D3325-90(2020)(Practice)
Standard Practice for Preservation of Waterborne Oil Samples

ABSTRACT
This practice establishes the standard method of preserving waterborne oil samples from the time of collection to the time of analysis. Information is provided to ensure sample integrity and to avoid contamination and to minimize microbial degradation. This practice is for controlled field or laboratory conditions and specifies thorough preparation of equipment and precise operation. If, however, these details must be compromised in a field emergency, nonstandard simplifications that will minimize or eliminate consequent errors are recommended. This procedure requires the use of the following apparatuses: sample containers, preferably borosilicate glass (plastic and metal are not acceptable ); closures; an explosion-proof refrigerator; and shipping containers (sturdy cartons or wooden boxes). Samples may be of several types, such as tar balls, collected oil, oil-water mixtures, emulsions, and oil and water on collecting devices such as silanized glass cloth, TFE-fluorocarbon polymer, or other materials. Instructions are given for the care of samples to minimize changes due to autoxidation and microbial attack between the time of sampling and the time of testing. Services available for transportation of samples are described as well.
SCOPE
1.1 This practice covers the preservation of waterborne oil samples from the time of collection to the time of analysis. Information is provided to ensure sample integrity and to avoid contamination and to minimize microbial degradation.  
1.2 The practice is for controlled field or laboratory conditions and specifies thorough preparation of equipment and precise operation. Where these details must be compromised in a field emergency, nonstandard simplifications are recommended that will minimize or eliminate consequent errors.  
Note 1: Procedures for the analysis of oil spill samples are Practices D3326, D3415, and D4489, and Test Methods D3650, D3327, D3328, and D3414. A guide to the use of ASTM test methods for the analysis of oil spill samples is found in Practice D3415.  
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.  
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ASTM D3415-98(2017)(Practice)
Standard Practice for Identification of Waterborne Oils

SIGNIFICANCE AND USE
4.1 Oil from one crude oil field is readily distinguishable from another, and differences in the makeup of oils from the same crude oil field can often be observed as well. Refined oils are fractions from crude oil stocks, usually derived from distillation processes. Two refined oils of the same type differ because of dissimilarities in the characteristics of their crude oil feed stocks as well as variations in refinery processes and any subsequent contact with other oils mixed in during transfer operations from residues in tanks, ships, pipes, hoses, and so forth. Thus, all petroleum oils, to some extent, have chemical compositions different from each other.  
4.2 Identification of a recovered oil is determined by comparison with known oils selected because of their possible relationship to the particular recovered oil, for example, suspected sources. Thus, samples of such known oils must be collected and submitted along with the unknown for analysis. Identification of the source of an unknown oil by itself cannot be made without comparison to a known oil. The principles of oil spill identification are discussed in Ref (1).4  
4.3 Many similarities (within uncertainties of sampling, analysis and weathering) will be needed to establish the identity beyond a reasonable doubt. The analyses described will distinguish many, but not all samples. Examples of weathering of various classes of oils are included in Ref (2).  
4.4 This practice is a guide to the use of ASTM test methods for the analysis of oil samples for oil spill identification purposes. The evaluation of results from analytical methods and preparation of an Oil Spill Identification Report are discussed in this practice. Other analytical methods are described in Ref (3).  
4.5 A quality assurance program for oil spill identification is specified.
SCOPE
1.1 This practice covers the broad concepts of sampling and analyzing waterborne oils for identification and comparison with suspected source oils. Detailed procedures are referenced in this practice. A general approach is given to aid the investigator in planning a program to solve the problem of chemical characterization and to determine the source of a waterborne oil sample.  
1.2 This practice is applicable to all waterborne oils taken from water bodies, either natural or man-made, such as open oceans, estuaries or bays, lakes, rivers, smaller streams, canals; or from beaches, marshes, or banks lining or edging these water systems. Generally, the waterborne oils float on the surface of the waters or collect on the land surfaces adjoining the waters, but occasionally these oils, or portions, are emulsified or dissolved in the waters, or are incorporated into the sediments underlying the waters, or into the organisms living in the water or sediments.  
1.3 This practice as presently written proposes the use of specific analytical techniques described in the referenced ASTM standards. As additional techniques for characterizing waterborne oils are developed and written up as test methods, this practice will be revised.  
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.  
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ASTM D3326-07(2017)(Practice)
Standard Practice for Preparation of Samples for Identification of Waterborne Oils

SIGNIFICANCE AND USE
4.1 Identification of a recovered oil is determined by comparison with known oils selected because of their possible relationship to the particular recovered oil, for example, suspected or questioned sources. Thus, samples of such known oils must be collected and submitted along with the unknown for analysis. It is unlikely that identification of the sources of an unknown oil by itself can be made without direct matching, that is, solely with a library of analyses.
SCOPE
1.1 This practice covers the preparation for analysis of waterborne oils recovered from water. The identification is based upon the comparison of physical and chemical characteristics of the waterborne oils with oils from suspect sources. These oils may be of petroleum or vegetable/animal origin, or both. Seven procedures are given as follows:    
Sections  
Procedure A (for samples of more than 50-mL volume containing significant quantities of hydrocarbons with boiling points above 280°C)  
8 to 12  
Procedure B (for samples containing significant quantities of hydrocarbons with boiling points above 280°C)  
13 to 17  
Procedure C (for waterborne oils containing significant amounts of components boiling below 280°C and to mixtures of these and higher boiling components)  
18 to 22  
Procedure D (for samples containing both petroleum and vegetable/animal derived oils)  
23 to 27  
Procedure E (for samples of light crudes and medium distillate fuels)  
28 to 34  
Procedure F (for thin films of oil-on-water)  
35 to 39  
Procedure G (for oil-soaked samples)  
40 to 44  
1.2 Procedures for the analytical examination of the waterborne oil samples are described in Practice D3415 and Test Methods D3328, D3414, and D3650. Refer to the individual oil identification test methods for the sample preparation method of choice. The deasphalting effects of the sample preparation method should be considered in selecting the best methods.  
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ASTM D1093-23(Test Method)
Standard Test Method for Acidity of Hydrocarbon Liquids and Their Distillation Residues

SIGNIFICANCE AND USE
5.1 Some petroleum products are treated with mineral acid as part of the refining procedure. Obviously, any residual mineral acid in a petroleum product is undesirable. The absence of a positive indication in the test for acidity of the distillation residue or aqueous extract of a hydrocarbon liquid is an assurance of the care used in refining the fuel or solvent.
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Standard Test Method for Qualitative Analysis for Active Sulfur Species in Fuels and Solvents (Doctor Test)

SIGNIFICANCE AND USE
5.1 Sulfur present as mercaptans or as hydrogen sulfide in distillate fuels and solvents can attack many metallic and non-metallic materials in fuel and other distribution systems. A negative result in the doctor test ensures that the concentration of these compounds is insufficient to cause such problems in normal use.
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ASTM D6300-23(Practice)
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SIGNIFICANCE AND USE
5.1 ASTM test methods are frequently intended for use in the manufacture, selling, and buying of materials in accordance with specifications and therefore should provide such precision that when the test is properly performed by a competent operator, the results will be found satisfactory for judging the compliance of the material with the specification. Statements addressing precision and bias are required in ASTM test methods. These then give the user an idea of the precision of the resulting data and its relationship to an accepted reference material or source (if available). Statements addressing determinability are sometimes required as part of the test method procedure in order to provide early warning of a significant degradation of testing quality while processing any series of samples.  
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1.1 This practice covers the necessary preparations and planning for the conduct of interlaboratory programs for the development of estimates of precision (determinability, repeatability, and reproducibility) and of bias (absolute and relative), and further presents the standard phraseology for incorporating such information into standard test methods.  
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SIGNIFICANCE AND USE
4.1 This test method provides a means of monitoring the sulfur level of various petroleum products and additives. This knowledge can be used to predict performance, handling, or processing properties. In some cases the presence of sulfur compounds is beneficial to the product and monitoring the depletion of sulfur can provide useful information. In other cases the presence of sulfur compounds is detrimental to the processing or use of the product.
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1.1 This test method covers procedures for the determination of total sulfur in petroleum products including lubricating oils containing additives, and in additive concentrates. This test method is applicable to samples boiling above 177 °C (350 °F). Other sulfur concentrations outside of those listed in 1.1.1 and 1.1.2 may be analyzed, but the precision stated may or may not apply. These procedures use IR detection or TCD following combustion in a furnace.  
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1.1.2 Procedure B, TCD Detection:  
1.1.2.1 This procedure is applicable to samples containing a mass fraction of sulfur between 0.071 % and 25.8 %.
1.1.2.2 Petroleum coke containing a mass fraction of sulfur between 0.19 % to 6.38 % sulfur may be analyzed.  
1.2 Petroleum coke containing a mass fraction of sulfur between 2.53 % to 3.79 % sulfur may be analyzed. Other sulfur concentrations may be analyzed, but the precision stated may or may not apply.
Note 1: The D1552 – 08 (2014) version of this standard contained two other procedures using iodate titrations. Since these procedures are no longer being used in the industry laboratories based on a survey of D02.SC 3 laboratories conducted in September 2014, they are being deleted. For earlier information on the deleted procedures, D1552 – 08 (2014) may be perused.  
1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
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 Test Method for Ultraviolet Absorbance and Absorptivity of Petroleum Products

SIGNIFICANCE AND USE
5.1 The absorbance of liquids and the absorptivity of liquid and solids at specified wavelengths in the ultraviolet are useful in characterizing petroleum products.
SCOPE
1.1 This test method covers the measurement of the ultraviolet absorption of a variety of petroleum products. It covers the absorbance of liquids or the absorptivity of liquids and solids, or both, at wavelengths in the region from 220 nm to 400 nm of the spectrum.  
1.2 The use of this test method implies that the conditions of measurement—wavelength, solvent (if any), sample path length, and sample concentration—are specified by reference to one of the examples of the application of this test method in the annexes or by a statement of other conditions of measurement.  
1.3 Examples of the application of this test method are the absorptivity of refined petroleum wax, and the absorptivity of USP petrolatum.  
1.4 The values stated in SI units are to be regarded as the standard. The values stated in Fahrenheit, feet, and inches, indicated in parentheses, are for information only.  
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 warning statements, see 7.3.1, 7.3.3, and 13.4.  
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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SIGNIFICANCE AND USE
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4.1.1 The word ‘customer’ can refer to both customers internal and external to the laboratory or organization.
SCOPE
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