ASTM D7419-13
(Test Method)Standard Test Method for Determination of Total Aromatics and Total Saturates in Lube Basestocks by High Performance Liquid Chromatography (HPLC) with Refractive Index Detection
Standard Test Method for Determination of Total Aromatics and Total Saturates in Lube Basestocks by High Performance Liquid Chromatography (HPLC) with Refractive Index Detection
SIGNIFICANCE AND USE
5.1 The composition of a lubricating oil has a large effect on the characteristics and uses of the oil. The determination of saturates, aromatics and polars is a key analysis of this composition. The characterization of the composition of lubricating oils is important in determining their interchangeability for use in blending etcetera.
SCOPE
1.1 This test method covers the determination of total aromatics and total saturates in additive-free lube basestocks using high performance liquid chromatography (HPLC) with refractive index (RI) detection. This test method is applicable to samples containing total aromatics in the concentration range of 0.2 to 46 mass %.
1.1.1 Polar compounds, if present, are combined with the total aromatics. Precision was determined for basestocks with polars content
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 and health practices and determine the applicability of regulatory limitations prior to use.
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Designation: D7419 − 13
Standard Test Method for
Determination of Total Aromatics and Total Saturates in
Lube Basestocks by High Performance Liquid
1
Chromatography (HPLC) with Refractive Index Detection
This standard is issued under the fixed designation D7419; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope* 3.1.1 aromatics, n—in high performance liquid
chromatography, aromatic hydrocarbon components, minus
1.1 This test method covers the determination of total
polarmaterial,thathasalongerretentiontimethansaturateson
aromatics and total saturates in additive-free lube basestocks
the specified polar columns, but can be removed as a single
using high performance liquid chromatography (HPLC) with
peak by backflushing the columns with heptane.
refractive index (RI) detection. This test method is applicable
3.1.1.1 Discussion—Generally, aromatic hydrocarbons con-
to samples containing total aromatics in the concentration
tain 1 to 4 rings.
range of 0.2 to 46 mass%.
3.1.2 backflush, v—elutionoftheHPLCmobilephaseinthe
1.1.1 Polar compounds, if present, are combined with the
backward or reverse direction from the silica gel column
total aromatics. Precision was determined for basestocks with
towards the cyano column.
polars content < 1.0 mass%.
3.1.2.1 Discussion—In this test method, it is used to elute
1.2 The values stated in SI units are to be regarded as
the total aromatics plus polars as one sharp component.
standard. No other units of measurement are included in this
3.1.3 foreflush, v—elution of HPLC mobile phase in the
standard.
forward direction.
1.3 This standard does not purport to address all of the
3.1.3.1 Discussion—In this test method, the sample enters
safety concerns, if any, associated with its use. It is the
the cyano column first followed by elution through the silica
responsibility of the user of this standard to establish appro-
gel column.
priate safety and health practices and determine the applica-
3.1.4 polars, n—in high performance liquid
bility of regulatory limitations prior to use.
chromatography, components that may contain organically
2. Referenced Documents
bonded nitrogen, oxygen and oxidized sulfur components and
2
are more strongly retained than aromatic hydrocarbons.
2.1 ASTM Standards:
3.1.4.1 Discussion—In this HPLC method, polars are back-
D4057Practice for Manual Sampling of Petroleum and
flushedwiththearomaticsandthetwocannotbedistinguished.
Petroleum Products
Generally present in very small amounts, such as < 1 mass%.
D4177Practice for Automatic Sampling of Petroleum and
Petroleum Products
3.1.5 saturates, n—hydrocarbon components that are not
D6299Practice for Applying Statistical Quality Assurance
retained strongly by the specified polar columns when heptane
and Control Charting Techniques to Evaluate Analytical
is used as the mobile phase.
Measurement System Performance
3.1.5.1 Discussion—Generally, these consist of paraffins
and cycloparaffins.
3. Terminology
3.1 Definitions:
4. Summary of Test Method
4.1 Aknown mass of sample is diluted in the mobile phase
1
This test method is under the jurisdiction of ASTM Committee D02 on
and a fixed volume of this solution is injected into a calibrated
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
high performance liquid chromatograph. The separation col-
Subcommittee D02.04.0C on Liquid Chromatography.
umn set has little affinity for the saturates while retarding the
Current edition approved May 1, 2013. Published June 2013. Originally
aromatic hydrocarbons and the polars. As a result of this
approved in 2007. Last previous edition approved in 2007 as D7419–07. DOI:
10.1520/D7419-13.
retardation,thearomatichydrocarbonsandpolarsareseparated
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
fromthesaturates.Atapredeterminedtime,aftertheelutionof
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
the saturates, the column is backflushed to elute the aromatics
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. and polars as a single sharp band.
*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 ----------------------
D7419 − 13
4.2 The column set is connected to a refractive index 6.5.1 UV-Detector—An optional but recommended UV de-
detector that detects the components as they elute from the tectorsettowavelength254nmmaybeusedinser
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D7419 − 07 D7419 − 13
Standard Test Method for
Determination of Total Aromatics and Total Saturates in
Lube Basestocks by High Performance Liquid
1
Chromatography (HPLC) with Refractive Index Detection
This standard is issued under the fixed designation D7419; 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 Scope*
1.1 This test method covers the determination of total aromatics and total saturates in additive-free lube basestocks using high
performance liquid chromatography (HPLC) with refractive index (RI) detection. This test method is applicable to samples
containing total aromatics in the concentration range of 0.2 to 46 mass %.
1.1.1 Polar compounds, if present, are combined with the total aromatics. Precision was determined for basestocks with polars
content < 1.0 mass %.
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 and health practices and determine the applicability of regulatory
limitations prior to use.
2. Referenced Documents
2
2.1 ASTM Standards:
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4177 Practice for Automatic Sampling of Petroleum and Petroleum Products
D6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measure-
ment System Performance
3. Terminology
3.1 Definitions:
3.1.1 aromatics, n—in high performance liquid chromatography, aromatic hydrocarbon components, minus polar material, that
has a longer retention time than saturates on the specified polar columns, but can be removed as a single peak by backflushing the
columns with heptane.
1
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.04.0C
on Liquid Chromatography.
Current edition approved Dec. 1, 2007May 1, 2013. Published February 2008June 2013. Originally approved in 2007. Last previous edition approved in 2007 as
D7419 – 07. DOI: 10.1520/D7419-07.10.1520/D7419-13.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3.1.1.1 Discussion—
Generally, aromatic hydrocarbons contain 1 to 4 rings.
3.1.2 backflush, v—elution of the HPLC mobile phase in the backward or reverse direction from the silica gel column towards
the cyano column.
3.1.2.1 Discussion—
In this test method, it is used to elute the total aromatics plus polars as one sharp component.
3.1.3 foreflush, v—elution of HPLC mobile phase in the forward direction.
*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 ----------------------
D7419 − 13
3.1.3.1 Discussion—
In this test method, the sample enters the cyano column first followed by elution through the silica gel column.
3.1.4 polars, n—in high performance liquid chromatography, components that may contain organically bonded nitrogen,
oxygen and oxidized sulfur components and are more strongly retained than aromatic hydrocarbons.
3.1.4.1 Discussion—
In this HPLC method, polars are backflushed with the aromatics and the two cannot be distinguished. Generally present in very
small amounts, such as < 1 mass %.
3.1.5 saturates, n—hydrocarbon components that are not retained strongly by the specified polar columns when heptane is used
as the mobile phase.
3.1.5.1 Discussion—
Generally, these consist of paraffins and cycloparaffins.
4. Summary of Test Method
4.1 A known mass of sample is diluted in the mobile phase and a fixed volume of this solution is injected into a calibrated high
performance liquid chromatograph. The separation column set has little affinity for the saturates while retarding the aromatic
hydrocarbons and the polars. As a result of this retardation, the aromatic hydrocarbons and polars are separa
...
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