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ASTM D6591-06

(Test Method)

Standard Test Method for Determination of Aromatic Hydrocarbon Types in Middle Distillates-High Performance Liquid Chromatography Method with Refractive Index Detection

Standard Test Method for Determination of Aromatic Hydrocarbon Types in Middle Distillates-High Performance Liquid Chromatography Method with Refractive Index Detection

SIGNIFICANCE AND USE
The aromatic hydrocarbon content of motor diesel fuel is a factor that can affect exhaust emissions and fuel combustion characteristics, as measured by cetane number.
The United States Environmental Protection Agency (US EPA) regulates the aromatic content of diesel fuels. California Air Resources Board (CARB) regulations place limits on the total aromatics content and polynuclear aromatic hydrocarbon content of motor diesel fuel, thus requiring an appropriate analytical determination to ensure compliance with the regulations.
This test method is applicable to materials in the same boiling range as motor diesel fuels and is unaffected by fuel coloration. Test Method D 1319, which has been mandated by the US EPA for the determination of aromatics in motor diesel fuel, excludes materials with final boiling points greater than 315°C (600°F) from its scope. Test Method D 2425 is applicable to the determination of both total aromatics and polynuclear aromatic hydrocarbons in diesel fuel, but is much more costly and time-consuming to perform. Test Method D 5186, currently specified by CARB, is also applicable to the determination of both total aromatics and polynuclear aromatic hydrocarbons in diesel fuel. Test Method D 5186, however, specifies the use of supercritical fluid chromatography equipment that may not be readily available.
Note 2—Test Method D 5186 was previously specified by CARB as an alternative to Test Method D 1319.
SCOPE
1.1 This test method covers a high performance liquid chromatographic test method for the determination of mono-aromatic, di-aromatic, tri+-aromatic, and polycyclic aromatic hydrocarbon contents in diesel fuels and petroleum distillates boiling in the range from 150 to 400°C. The total aromatic content in % m/m is calculated from the sum of the corresponding individual aromatic hydrocarbon types.Note 1
Aviation fuels and petroleum distillates with a boiling point range from 50 to 300°C are not determined by this test method and should be analyzed by Test Method, D 6379 or other suitable equivalent test methods.
1.2 The precision of this test method has been established for diesel fuels and their blending components, containing from 4 to 40 % (m/m) mono-aromatic hydrocarbons, 0 to 20 % (m/m) di-aromatic hydrocarbons, 0 to 6 % (m/m) tri+-aromatic hydrocarbons, 0 to 26 % (m/m) polycyclic aromatic hydrocarbons, and 4 to 65 % (m/m) total aromatic hydrocarbons.
1.3 Compounds containing sulfur, nitrogen, and oxygen are possible interferents. Mono-alkenes do not interfere, but conjugated di- and poly-alkenes, if present, are possible interferents.
1.4 By convention, this standard defines the aromatic hydrocarbon types on the basis of their elution characteristics from the specified liquid chromatography column relative to model aromatic compounds. Quantification is by external calibration using a single aromatic compound, which may or may not be representative of the aromatics in the sample, for each aromatic hydrocarbon type. Alternative techniques and methods may classify and quantify individual aromatic hydrocarbon types differently.
1.5 Fatty Acid Methyl Esters (FAME), if present, interfere with tri+-aromatic hydrocarbons. If this method is used for diesel containing FAME, the amount of tri+-aromatics will be over estimated.
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.

General Information

Status
Historical
Publication Date
31-Oct-2006
ICS
71.040.50 - Physicochemical methods of analysis
Technical Committee
D02 - Petroleum Products, Liquid Fuels, and Lubricants
Drafting Committee
D02.04.0C - Liquid Chromatography
Current Stage
Ref Project

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ASTM D6591-06 - Standard Test Method for Determination of Aromatic Hydrocarbon Types in Middle Distillates-High Performance Liquid Chromatography Method with Refractive Index DetectionASTM D6591-06 - Standard Test Method for Determination of Aromatic Hydrocarbon Types in Middle Distillates-High Performance Liquid Chromatography Method with Refractive Index Detection
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ASTM D6591-06 - Standard Test Method for Determination of Aromatic Hydrocarbon Types in Middle Distillates-High Performance Liquid Chromatography Method with Refractive Index Detection
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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: D6591 – 06
Designation: 548/06
Standard Test Method for
Determination of Aromatic Hydrocarbon Types in Middle
Distillates—High Performance Liquid Chromatography
1
Method with Refractive Index Detection
This standard is issued under the fixed designation D6591; 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.
INTRODUCTION
This test method has the same title as IP 548-06 and is intended to be technically equivalent. The
ASTM format for test methods has been used, and where possible, equivalent ASTM test methods
have replaced the IP or ISO standards.
The test method is intended to be used as one of several possible alternative instrumental test
methods that are aimed at quantitative determination of hydrocarbon types in fuels. This does not
imply that a correlation necessarily exists between this and any other test method intended to give this
information, and it is the responsibility of the user to determine such correlation if necessary.
1. Scope* 1.3 Compounds containing sulfur, nitrogen, and oxygen are
possible interferents. Mono-alkenes do not interfere, but con-
1.1 This test method covers a high performance liquid
jugated di- and poly-alkenes, if present, are possible interfer-
chromatographic test method for the determination of mono-
ents.
aromatic, di-aromatic, tri+-aromatic, and polycyclic aromatic
1.4 By convention, this standard defines the aromatic hy-
hydrocarbon contents in diesel fuels and petroleum distillates
drocarbon types on the basis of their elution characteristics
boiling in the range from 150 to 400°C. The total aromatic
from the specified liquid chromatography column relative to
content in % m/m is calculated from the sum of the corre-
model aromatic compounds. Quantification is by external
sponding individual aromatic hydrocarbon types.
calibration using a single aromatic compound, which may or
NOTE 1—Aviation fuels and petroleum distillates with a boiling point
may not be representative of the aromatics in the sample, for
range from 50 to 300°C are not determined by this test method and should
each aromatic hydrocarbon type. Alternative techniques and
be analyzed by Test Method, D6379 or other suitable equivalent test
methods may classify and quantify individual aromatic hydro-
methods.
carbon types differently.
1.2 The precision of this test method has been established
1.5 Fatty Acid Methyl Esters (FAME), if present, interfere
for diesel fuels and their blending components, containing
with tri+-aromatic hydrocarbons. If this method is used for
from 4 to 40 % (m/m) mono-aromatic hydrocarbons, 0 to 20 %
diesel containing FAME, the amount of tri+-aromatics will be
(m/m) di-aromatic hydrocarbons, 0 to 6 % (m/m) tri+-aromatic
over estimated.
hydrocarbons, 0 to 26 % (m/m) polycyclic aromatic hydrocar-
1.6 This standard does not purport to address all of the
bons, and 4 to 65 % (m/m) total aromatic hydrocarbons.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
1
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee 2. Referenced Documents
D02.04.0C on Liquid Chromatography.
2
2.1 ASTM Standards:
This test method is based on material published in IP Standard Methods for
D1319 Test Method for Hydrocarbon Types in Liquid
Analysis and Testing of Petroleum and Related Products and British Standard 2000
Parts, copyright The Institute of Petroleum, 61 New Cavendish Street, London
Petroleum Products by Fluorescent Indicator Adsorption
W1M 8AR. Adapted with permission of The Institute of Petroleum.
D2425 Test Method for Hydrocarbon Types in Middle
Current edition approved Nov. 1, 2006. Published December 2006. Originally
Distillates by Mass Spectrometry
approved in 2000. Last previous edition approved in 2000 as D6591 – 00. DOI:
10.1520/D6591-06.
*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.
1

---------------------- Page: 1 ----------------------
D6591 – 06
D4057 Practice for Manual Sampling of Petroleum and phenanthrenes, pyrenes, fluoranthenes, chrysenes, triph-
Petroleum Products enylenes, and benzanthracenes.
D4177 Practice for Automatic Sampling of Petroleum and
4. Summary of Test Method
Petroleum Products
4.1 Aknown mass of sample is diluted in the mobile pha
...

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5.1 ASTM standard gas chromatographic methods for the analysis of petroleum products require calibration of the gas chromatographic system by preparation and analysis of specified reference mixtures. Frequently, minimal information is given in these methods on the practice of calculating calibration or response factors. Test Methods D2268, D2427, D2804, D2998, D3329, D3362, D3465, D3545, and D3695 are examples. The present practice helps to fill this void by providing a detailed reference procedure for calculating response factors, as exemplified by analysis of a standard blend of C6 to C11 n-paraffins using n-C12 as the diluent.  
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Standard Test Method for Determination of Oxygenates, Benzene, Toluene, C8–C12 Aromatics and Total Aromatics in Finished Gasoline by Gas Chromatography/Fourier Transform Infrared Spectroscopy

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5.1 Test methods to determine oxygenates, benzene, and the aromatic content of gasoline are necessary to assess product quality and to meet new fuel regulations.  
5.2 This test method can be used for gasolines that contain oxygenates (alcohols and ethers) as additives. It has been determined that the common oxygenates found in finished gasoline do not interfere with the analysis of benzene and other aromatics by this test method.
SCOPE
1.1 This test method covers the quantitative determination of oxygenates: methyl-t-butylether (MTBE), di-isopropyl ether (DIPE), ethyl-t-butylether (ETBE), t-amylmethyl ether (TAME), methanol (MeOH), ethanol (EtOH), 2-propanol (2-PrOH), t-butanol (t-BuOH), 1-propanol (1-PrOH), 2-butanol (2-BuOH), i-butanol (i-BuOH), 1-butanol (1-BuOH); benzene, toluene and C8–C12 aromatics, and total aromatics in finished motor gasoline by gas chromatography/Fourier Transform infrared spectroscopy (GC/FTIR).  
1.2 This test method covers the following concentration ranges: 0.1 % to 20 % by volume per component for ethers and alcohols; 0.1 % to 2 % by volume benzene; 1 % to 15 % by volume for toluene, 10 % to 40 % by volume total (C6–C12) aromatics.  
1.3 The method has not been tested by ASTM for refinery individual hydrocarbon process streams, such as reformates, fluid catalytic cracking naphthas, etc., used in blending of gasolines.  
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5.1 The determination of the boiling point distribution of crude oils and vacuum residues, as well as other petroleum fractions, yields important information for refinery operation. These boiling point distributions provide information as to the potential mass percent yield of products. This test method may provide useful information that can aid in establishing operational conditions in the refinery. Knowledge of the amount of residue produced is important in determining the economics of the refining process.
SCOPE
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Standard Test Method for Analysis of Barium, Calcium, Magnesium, and Zinc in Unused Lubricating Oils by Atomic Absorption Spectrometry

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5.1 Some oils are formulated with metal-containing additives that act as detergents, antioxidants, antiwear agents, etc. Some of these additives contain one or more of these metals: barium, calcium, zinc, and magnesium. This test method provides a means of determining the concentration of these metals that gives an indication of the additive content in these oils.  
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4.1 If ASTM Committee E13 has not specified an appropriate test procedure for a specific type of instrument, or if the sample specified by a Committee E13 procedure is incompatible with the intended instrument operation, then this practice can be used to develop practical performance tests.  
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1.1 This practice covers basic procedures that can be used to develop instrument performance tests for spectroscopic based online, at-line, laboratory and field analyzers. The practice is intended to be applicable to Raman spectrometers and to infrared spectrophotometers operating in the near-infrared and mid-infrared regions.  
1.2 This practice is not intended as a replacement for specific practices, such as Practices E275, E925, E932, E958, E1421, or E1683 that exist for measuring performance of specific types of laboratory spectroscopic instruments. Instead, this practice is intended to provide guidelines as to how similar practices should be developed when specific practices do not exist for a particular instrument type, or when specific practices are not applicable due to sampling or safety concerns. This practice can be used to develop instrument performance tests for on-line process spectroscopic-based analyzers.  
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1.2.2 Instrument performance tests do not typically evaluate performance of analyzer sampling systems.  
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ASTM D6277-07(2022)(Test Method)
Standard Test Method for Determination of Benzene in Spark-Ignition Engine Fuels Using Mid Infrared Spectroscopy

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5.1 Benzene is a compound that endangers health, and the concentration is limited by environmental protection agencies to produce a less toxic gasoline.  
5.2 This test method is fast, simple to run, and inexpensive.  
5.3 This test method is applicable for quality control in the production and distribution of spark-ignition engine fuels.
SCOPE
1.1 This test method covers the determination of the percentage of benzene in spark-ignition engine fuels. It is applicable to concentrations from 0.1 % to 5 % by volume.  
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 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 D6296-22(Test Method)
Standard Test Method for Total Olefins in Spark-ignition Engine Fuels by Multidimensional Gas Chromatography

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5.1 The quantitative determination of olefins in spark-ignition engine fuels is required to comply with government regulations.  
5.2 Knowledge of the total olefin content provides a means to monitor the efficiency of catalytic cracking processes.  
5.3 This test method provides better precision for olefin content than Test Method D1319. It also provides data in a much shorter time, approximately 20 min following calibration, and maximizes automation to reduce operator labor.  
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1.1 This test method provides for the quantitative determination of total olefins in the C4 to C10 range in spark-ignition engine fuels or related hydrocarbon streams, such as naphthas and cracked naphthas. Olefin concentrations in the range from 0.2 % by liquid-volume or mass to 5.0 % by liquid-volume or mass, or both, can be determined directly on the as-received sample whereas olefins in samples containing higher concentrations are determined after appropriate sample dilution prior to analysis.  
1.2 This test method is applicable to samples containing alcohols and ethers; however, samples containing greater than 15 % alcohol must be diluted. Samples containing greater than 5.0 % ether must also be diluted to the 5.0 % or less level, prior to analysis. When ethyl-tert-butylether is present, only olefins in the C4 to C9 range can be determined.  
1.3 This test method can not be used to determine individual olefin components.  
1.4 This test method can not be used to determine olefins having higher carbon numbers than C10.
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1.5 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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Standard Test Method for Determination of Aromatic Hydrocarbon Types in Aviation Fuels and Petroleum Distillates—High Performance Liquid Chromatography Method with Refractive Index Detection

SIGNIFICANCE AND USE
5.1 Accurate quantitative information on aromatic hydrocarbon types can be useful in determining the effects of petroleum processes on production of various finished fuels. This information can also be useful for indicating the quality of fuels and for assessing the relative combustion properties of finished fuels.
SCOPE
1.1 This test method covers a high performance liquid chromatographic test method for the determination of mono-aromatic and di-aromatic hydrocarbon contents in aviation kerosenes and petroleum distillates boiling in the range from 50 °C to 300 °C, such as Jet A or Jet A-1 fuels. The total aromatic content is calculated from the sum of the individual aromatic hydrocarbon-types.  
Note 1: Samples with a final boiling point greater than 300 °C that contain tri-aromatic and higher polycyclic aromatic compounds are not determined by this test method and should be analyzed by Test Method D6591 or other suitable equivalent test methods.  
1.2 This test method is applicable to distillates containing from 0.8 % to 44.0 % by mass mono-aromatic hydrocarbons, 0.23 % to 6.20 % by mass di-aromatic hydrocarbons, and 0.7 % to 50 % by mass total aromatics. Although this method generates results in m/m, results may also be quoted in v/v.  
1.3 The precision of this test method has been established for kerosene boiling range distillates containing from 0.40 % to 44.0 % by mass mono-aromatic hydrocarbons, 0.02 % to 6.20 % by mass di-aromatic hydrocarbons, and 0.40 % to 50.0 % by mass total aromatics. If results are quoted in volume, the precision is 0.3 % to 41.4 % by volume mono-aromatics, 0.01 % to 5.00 % by volume di-aromatics, and 0.30 % to 46.3 % by volume total aromatics. As calculated by IP 367-1.  
1.4 Compounds containing sulfur, nitrogen, and oxygen are possible interferents. Mono-alkenes do not interfere, but conjugated di- and poly-alkenes, if present, are possible interferents.  
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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