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ASTM D3415-98(2024)

(Practice)

Standard Practice for Identification of Waterborne Oils

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.  
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-Mar-2024
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

Replaces
ASTM D3415-98(2017) - Standard Practice for Identification of Waterborne Oils
Effective Date
01-Apr-2024
Refers
ASTM D3326-07(2024) - Standard Practice for Preparation of Samples for Identification of Waterborne Oils
Effective Date
01-Apr-2024
Refers
ASTM D3326-07(2017) - Standard Practice for Preparation of Samples for Identification of Waterborne Oils
Effective Date
15-Dec-2017
Refers
ASTM D4489-95(2017) - Standard Practices for Sampling of Waterborne Oils
Effective Date
15-Dec-2017
Referred By
ASTM D3325-90(2020) - Standard Practice for Preservation of Waterborne Oil Samples
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 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-Apr-2024
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 D4489-95(2024) - Standard Practices for Sampling of Waterborne Oils
Effective Date
01-Apr-2024

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ASTM D3415-98(2024) - Standard Practice for Identification of Waterborne Oils
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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: D3415 − 98 (Reapproved 2024)
Standard Practice for
Identification of Waterborne Oils
This standard is issued under the fixed designation D3415; 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
2.1 ASTM Standards:
1.1 This practice covers the broad concepts of sampling and
D1129 Terminology Relating to Water
analyzing waterborne oils for identification and comparison
D3325 Practice for Preservation of Waterborne Oil Samples
with suspected source oils. Detailed procedures are referenced
D3326 Practice for Preparation of Samples for Identification
in this practice. A general approach is given to aid the
of Waterborne Oils
investigator in planning a program to solve the problem of
D3328 Test Methods for Comparison of Waterborne Petro-
chemical characterization and to determine the source of a
leum Oils by Gas Chromatography
waterborne oil sample.
D3414 Test Method for Comparison of Waterborne Petro-
1.2 This practice is applicable to all waterborne oils taken
leum Oils by Infrared Spectroscopy (Withdrawn 2018)
from water bodies, either natural or man-made, such as open
D3650 Test Method for Comparison of Waterborne Petro-
oceans, estuaries or bays, lakes, rivers, smaller streams, canals; leum Oils By Fluorescence Analysis (Withdrawn 2018)
or from beaches, marshes, or banks lining or edging these
D4489 Practices for Sampling of Waterborne Oils
water systems. Generally, the waterborne oils float on the D4840 Guide for Sample Chain-of-Custody Procedures
surface of the waters or collect on the land surfaces adjoining D5037 Test Method for Comparison of Waterborne Petro-
leum Oils by High Performance Liquid Chromatography
the waters, but occasionally these oils, or portions, are emul-
(Withdrawn 2002)
sified or dissolved in the waters, or are incorporated into the
D5739 Practice for Oil Spill Source Identification by Gas
sediments underlying the waters, or into the organisms living
Chromatography and Positive Ion Electron Impact Low
in the water or sediments.
Resolution Mass Spectrometry
1.3 This practice as presently written proposes the use of
E620 Practice for Reporting Opinions of Scientific or Tech-
specific analytical techniques described in the referenced
nical Experts
ASTM standards. As additional techniques for characterizing
waterborne oils are developed and written up as test methods,
3. Terminology
this practice will be revised.
3.1 Definitions:
1.4 This standard does not purport to address all of the
3.1.1 For definitions of terms used in this standard, refer to
safety concerns, if any, associated with its use. It is the
Terminology D1129, and to Practices D3325, D3326, D4489,
responsibility of the user of this standard to establish appro-
and D5739, and Test Methods D3328, D3650, and D5037.
priate safety, health, and environmental practices and deter-
3.2 Definitions of Terms Specific to This Standard:
mine the applicability of regulatory limitations prior to use.
3.2.1 waterborne oil, n—any oil, whether or not derived
1.5 This international standard was developed in accor-
from petroleum, carried by a water system (for example, ocean,
dance with internationally recognized principles on standard-
bay, lake, river, etc.) usually at the surface but occasionally
ization established in the Decision on Principles for the
emulsified or dissolved in the water. The waterborne oil can
Development of International Standards, Guides and Recom-
also be found on beaches or banks edging the water body, in
mendations issued by the World Trade Organization Technical the sediments underlying the water, or in the organisms living
Barriers to Trade (TBT) Committee.
in the water or in the sediments.
1 2
This practice is under the jurisdiction of ASTM Committee D19 on Water and For referenced ASTM standards, visit the ASTM website, www.astm.org, or
is the direct responsibility of Subcommittee D19.06 on Methods for Analysis for contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Organic Substances in Water. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved April 1, 2024. Published April 2024. Originally the ASTM website.
approved in 1975. Last previous edition approved in 2017 as D3415 – 98 (2017). The last approved version of this historical standard is referenced on
DOI: 10.1520/D3415-98R24. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D3415 − 98 (2024)
4. Significance and Use sample is analyzed with samples for each spill case. This
monitors both sample preparation and instrument performance.
4.1 Oil from one crude oil field is readily distinguishable
5.4.2 Remove an aliquot of one of the samples for each case
from another, and differences in the makeup of oils from the
prior to sample preparation and treat it as a separate sample.
same crude oil field can often be observed as well. Refined oils
This quality control (QC) sample should be taken from a spill
are fractions from crude oil stocks, usually derived from
sample if there is sufficient sample volume to do so. Otherwise,
distillation processes. Two refined oils of the same type differ
a suspected source sample may be used.
because of dissimilarities in the characteristics of their crude
5.4.3 Evaluate the data for the QC sample and its duplicate
oil feed stocks as well as variations in refinery processes and
aliquot according to the guidelines described for each Test
any subsequent contact with other oils mixed in during transfer
Method (refer to 5.5). If the data do not meet the criteria for a
operations from residues in tanks, ships, pipes, hoses, and so
match, investigate the problem. If there is a problem with one
forth. Thus, all petroleum oils, to some extent, have chemical
instrument, the analysis must be repeated for that test method
compositions different from each other.
after the problem is corrected. If there is a sample preparation
4.2 Identification of a recovered oil is determined by com-
problem, the analysis should be repeated after the problem is
parison with known oils selected because of their possible
identified.
relationship to the particular recovered oil, for example,
5.5 Analysis of Samples:
suspected sources. Thus, samples of such known oils must be
5.5.1 Analyze spill samples as well as any suspected source
collected and submitted along with the unknown for analysis.
oils, by gas chromatography (Test Method A or B of Test
Identification of the source of an unknown oil by itself cannot
Methods D3328, D3414) and by either infrared analysis (Test
be made without comparison to a known oil. The principles of
Methods D3414, D3650), or fluorescence spectroscopy (Test
oil spill identification are discussed in Ref (1).
Method D3650, Practices D4489). Interpretation of the
...

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ASTM D3326-07(2024)(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)  
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Procedure G (for oil-soaked samples)  
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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.  
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. Specific caution statements are given in Sections 6 and 32.  
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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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.  
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ASTM D3328-06(2020)(Test Method)
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.  
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ASTM D189-24(Test Method)
Standard Test Method for Conradson Carbon Residue of Petroleum Products

SIGNIFICANCE AND USE
5.1 The carbon residue value of burner fuel serves as a rough approximation of the tendency of the fuel to form deposits in vaporizing pot-type and sleeve-type burners. Similarly, provided alkyl nitrates are absent (or if present, provided the test is performed on the base fuel without additive) the carbon residue of diesel fuel correlates approximately with combustion chamber deposits.  
5.2 The carbon residue value of motor oil, while at one time regarded as indicative of the amount of carbonaceous deposits a motor oil would form in the combustion chamber of an engine, is now considered to be of doubtful significance due to the presence of additives in many oils. For example, an ash-forming detergent additive may increase the carbon residue value of an oil yet will generally reduce its tendency to form deposits.  
5.3 The carbon residue value of gas oil is useful as a guide in the manufacture of gas from gas oil, while carbon residue values of crude oil residuums, cylinder and bright stocks, are useful in the manufacture of lubricants.
SCOPE
1.1 This test method covers the determination of the amount of carbon residue (Note 1) left after evaporation and pyrolysis of an oil, and is intended to provide some indication of relative coke-forming propensities. This test method is generally applicable to relatively nonvolatile petroleum products which partially decompose on distillation at atmospheric pressure. Petroleum products containing ash-forming constituents as determined by Test Method D482 or IP Method 4 will have an erroneously high carbon residue, depending upon the amount of ash formed (Note 2 and Note 4).  
Note 1: The term carbon residue is used throughout this test method to designate the carbonaceous residue formed after evaporation and pyrolysis of a petroleum product under the conditions specified in this test method. The residue is not composed entirely of carbon, but is a coke which can be further changed by pyrolysis. The term carbon residue is continued in this test method only in deference to its wide common usage.
Note 2: Values obtained by this test method are not numerically the same as those obtained by Test Method D524. Approximate correlations have been derived (see Fig. X1.1), but need not apply to all materials which can be tested because the carbon residue test is applied to a wide variety of petroleum products.
Note 3: The test results are equivalent to Test Method D4530, (see Fig. X1.2).
Note 4: In diesel fuel, the presence of alkyl nitrates such as amyl nitrate, hexyl nitrate, or octyl nitrate causes a higher residue value than observed in untreated fuel, which can lead to erroneous conclusions as to the coke forming propensity of the fuel. The presence of alkyl nitrate in the fuel can be detected by Test Method D4046.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 WARNING—Mercury has been designated by many regulatory agencies as a hazardous substance that can cause serious medical issues. Mercury, or its vapor, has been demonstrated to be hazardous to health and corrosive to materials. Use caution when handling mercury and mercury-containing products. See the applicable product Safety Data Sheet (SDS) for additional information. The potential exists that selling mercury or mercury-containing products, or both, is prohibited by local or national law. Users must determine legality of sales in their location.  
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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.  
1.3 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 D445-24(Test Method)
Standard Test Method for Kinematic Viscosity of Transparent and Opaque Liquids (and Calculation of Dynamic Viscosity)

SIGNIFICANCE AND USE
5.1 Many petroleum products, and some non-petroleum materials, are used as lubricants, and the correct operation of the equipment depends upon the appropriate viscosity of the liquid being used. In addition, the viscosity of many petroleum fuels is important for the estimation of optimum storage, handling, and operational conditions. Thus, the accurate determination of viscosity is essential to many product specifications.
SCOPE
1.1 This test method specifies a procedure for the determination of the kinematic viscosity, ν, of liquid petroleum products, both transparent and opaque, by measuring the time for a volume of liquid to flow under gravity through a calibrated glass capillary viscometer. The dynamic viscosity, η, can be obtained by multiplying the kinematic viscosity, ν, by the density, ρ, of the liquid.  
Note 1: For the measurement of the kinematic viscosity and viscosity of bitumens, see also Test Methods D2170 and D2171.
Note 2: ISO 3104 corresponds to Test Method D445 – 03.  
1.2 The result obtained from this test method is dependent upon the behavior of the sample and is intended for application to liquids for which primarily the shear stress and shear rates are proportional (Newtonian flow behavior). If, however, the viscosity varies significantly with the rate of shear, different results may be obtained from viscometers of different capillary diameters. The procedure and precision values for residual fuel oils, which under some conditions exhibit non-Newtonian behavior, have been included.  
1.3 The range of kinematic viscosities covered by this test method is from 0.2 mm2/s to 300 000 mm2/s (see Table A1.1) at all temperatures (see 6.3 and 6.4). The precision has only been determined for those materials, kinematic viscosity ranges and temperatures as shown in the footnotes to the precision section.  
1.4 The values stated in SI units are to be regarded as standard. The SI unit used in this test method for kinematic viscosity is mm2/s, and the SI unit used in this test method for dynamic viscosity is mPa·s. For user reference, 1 mm2/s = 10-6 m2/s = 1 cSt and 1 mPa·s = 1 cP = 0.001 Pa·s.  
1.5 WARNING—Mercury has been designated by many regulatory agencies as a hazardous substance that can cause serious medical issues. Mercury, or its vapor, has been demonstrated to be hazardous to health and corrosive to materials. Use Caution when handling mercury and mercury-containing products. See the applicable product Safety Data Sheet (SDS) for additional information. The potential exists that selling mercury or mercury-containing products, or both, is prohibited by local or national law. Users must determine legality of sales in their location.  
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ASTM D6708-24(Practice)
Standard Practice for Statistical Assessment and Improvement of Expected Agreement Between Two Test Methods that Purport to Measure the Same Property of a Material

SIGNIFICANCE AND USE
5.1 This practice can be used to determine if a constant, proportional, or linear bias correction can improve the degree of agreement between two methods that purport to measure the same property of a material.  
5.2 The bias correction developed in this practice can be applied to a single result (X) obtained from one test method (method X) to obtain a predicted result ( Y^) for the other test method (method Y).
Note 5: Users are cautioned to ensure that  Y^ is within the scope of method Y before its use.  
5.3 The between methods reproducibility established by this practice can be used to construct an interval around  Y^ that would contain the result of test method Y, if it were conducted, with approximately 95 % probability.  
5.4 This practice can be used to guide commercial agreements and product disposition decisions involving test methods that have been evaluated relative to each other in accordance with this practice.  
5.5 The magnitude of a statistically detectable bias is directly related to the uncertainties of the statistics from the experimental study. These uncertainties are related to both the size of the data set and the precision of the processes being studied. A large data set, or, highly precise test method(s), or both, can reduce the uncertainties of experimental statistics to the point where the “statistically detectable” bias can become “trivially small,” or be considered of no practical consequence in the intended use of the test method under study. Therefore, users of this practice are advised to determine in advance as to the magnitude of bias correction below which they would consider it to be unnecessary, or, of no practical concern for the intended application prior to execution of this practice.
Note 6: It should be noted that the determination of this minimum bias of no practical concern is not a statistical decision, but rather, a subjective decision that is directly dependent on the application requirements of the users.
SCOPE
1.1 This practice covers statistical methodology for assessing the expected agreement between two different standard test methods that purport to measure the same property of a material, and for the purpose of deciding if a simple linear bias correction can further improve the expected agreement. It is intended for use with results obtained from interlaboratory studies meeting the requirement of Practice D6300 or equivalent (for example, ISO 4259). The interlaboratory studies shall be conducted on at least ten materials in common that among them span the intersecting scopes of the test methods, and results shall be obtained from at least six laboratories using each method. Requirements in this practice shall be met in order for the assessment to be considered suitable for publication in either method, if such publication includes claim to have been carried out in compliance with this practice. Any such publication shall include mandatory information regarding certain details of the assessment outcome as specified in the Report section of this practice.  
1.2 The statistical methodology is based on the premise that a bias correction will not be needed. In the absence of strong statistical evidence that a bias correction would result in better agreement between the two methods, a bias correction is not made. If a bias correction is required, then the parsimony principle is followed whereby a simple correction is to be favored over a more complex one.
Note 1: Failure to adhere to the parsimony principle generally results in models that are over-fitted and do not perform well in practice.  
1.3 The bias corrections of this practice are limited to a constant correction, proportional correction, or a linear (proportional + constant) correction.  
1.4 The bias-correction methods of this practice are method symmetric, in the sense that equivalent corrections are obtained regardless of which method is bias-corrected to match the othe...

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ASTM
ASTM D6300-24(Practice)
Standard Practice for Determination of Precision and Bias Data for Use in Test Methods for Petroleum Products, Liquid Fuels, and Lubricants

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.  
5.2 Repeatability and reproducibility are defined in the precision section of every Committee D02 test method. Determinability is defined above in Section 3. The relationship among the three measures of precision can be tabulated in terms of their different sources of variation (see Table 1).  
5.2.1 When used, determinability is a mandatory part of the Procedure section. It will allow operators to check their technique for the sequence of operations specified. It also ensures that a result based on the set of determined values is not subject to excessive variability from that source.  
5.3 A bias statement furnishes guidelines on the relationship between a set of test results and a related set of accepted reference values. When the bias of a test method is known, a compensating adjustment can be incorporated in the test method.  
5.4 This practice is intended for use by D02 subcommittees in determining precision estimates and bias statements to be used in D02 test methods. Its procedures correspond with ISO 4259 and are the basis for the Committee D02 computer software, Calculation of Precision Data: Petroleum Test Methods. The use of this practice replaces that of Re...
SCOPE
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.  
1.2 This practice is generally limited to homogeneous petroleum products, liquid fuels, and lubricants with which serious sampling problems (such as heterogeneity or instability) do not normally arise.  
1.3 This practice may not be suitable for products with sampling problems as described in 1.2, solid or semisolid products such as petroleum coke, industrial pitches, paraffin waxes, greases, or solid lubricants when the heterogeneous properties of the substances create sampling problems. In such instances, consult a trained statistician.  
1.4 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
ASTM D6749-24(Test Method)
Standard Test Method for Pour Point of Petroleum Products (Automatic Air Pressure Method)

SIGNIFICANCE AND USE
5.1 The pour point of a petroleum product is an index of the lowest temperature of its utility for certain applications. Flow characteristics, like pour point, can be critical for the correct operation of lubricating systems, fuel systems, and pipeline operations.  
5.2 Petroleum blending operations require precise measurement of the pour point.  
5.3 Test results from this test method can be determined at either 1 °C or 3 °C intervals.  
5.4 This test method yields a pour point in a format similar to Test Method D97/IP 15 when the 3 °C interval results are reported. However, when specification requires Test Method D97/IP 15, do not substitute this test method.
Note 2: Since some users may wish to report their results in a format similar to Test Method D97/IP 15 (in 3 °C intervals), the precision data were derived for the 3 °C intervals. For statements on bias relative to Test Method D97/IP 15, see 13.3.1.  
5.5 This test method has better repeatability and reproducibility relative to Test Method D97/IP 15 as measured in the 1998 interlaboratory test program (see Section 13).
SCOPE
1.1 This test method covers the determination of pour point of petroleum products by an automatic apparatus that applies a slightly positive air pressure onto the specimen surface while the specimen is being cooled.  
1.2 This test method is designed to cover the range of temperatures from −57 °C to +51 °C; however, the range of temperatures included in the (1998) interlaboratory test program only covered the temperature range from −51 °C to −11 °C.  
1.3 Test results from this test method can be determined at either 1 °C or 3 °C testing intervals.  
1.4 This test method is not intended for use with crude oils.
Note 1: The applicability of this test method on residual fuel samples has not been verified. For further information on the applicability, refer to 13.4.  
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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.  
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
ASTM D1500-24(Test Method)
Standard Test Method for ASTM Color of Petroleum Products (ASTM Color Scale)

SIGNIFICANCE AND USE
4.1 Determination of the color of petroleum products is used mainly for manufacturing control purposes and is an important quality characteristic, since color is readily observed by the user of the product. In some cases, the color may serve as an indication of the degree of refinement of the material. When the color range of a particular product is known, a variation outside the established range may indicate possible contamination with another product. However, color is not always a reliable guide to product quality and should not be used indiscriminately in product specifications.
SCOPE
1.1 This test method covers the visual determination of the color of a wide variety of petroleum products, such as lubricating oils, heating oils, diesel fuel oils, and petroleum waxes.  
Note 1: Test Method D156 is applicable to refined products that have an ASTM color lighter than 0.5.
Note 2: The color of some dyed products may extend outside color range defined by the glass reference standards employed in the testing procedure. Furthermore, samples used to determine the precision and bias did not include dyed products.
Note 3: It is up to the user to determine the suitability of this test method for their dyed products.  
1.2 This test method reports results specific to the test method and recorded as “ASTM Color.”  
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.  
1.4 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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