ASTM D2887-23

Standard Test Method for Boiling Range Distribution of Petroleum Fractions by Gas Chromatography

SIGNIFICANCE AND USE
5.1 The boiling range distribution of petroleum fractions provides an insight into the composition of feedstocks and products related to petroleum refining processes. The gas chromatographic simulation of this determination can be used to replace conventional distillation methods for control of refining operations. This test method can be used for product specification testing with the mutual agreement of interested parties.  
5.2 Boiling range distributions obtained by this test method are essentially equivalent to those obtained by true boiling point (TBP) distillation (see Test Method D2892). They are not equivalent to results from low efficiency distillations such as those obtained with Test Method D86 or D1160.  
5.3 Procedure B was tested with biodiesel mixtures and reports the Boiling Point Distribution of FAME esters of vegetable and animal origin mixed with ultra low sulfur diesel.
SCOPE
1.1 This test method covers the determination of the boiling range distribution of petroleum products. The test method is applicable to petroleum products and fractions having a final boiling point of 538 °C (1000 °F) or lower at atmospheric pressure as measured by this test method. This test method is limited to samples having a boiling range greater than 55.5 °C (100 °F), and having a vapor pressure sufficiently low to permit sampling at ambient temperature.
Note 1: Since a boiling range is the difference between two temperatures, only the constant of 1.8 °F/°C is used in the conversion of the temperature range from one system of units to another.  
1.1.1 Procedure A (Sections 6 – 14)—Allows a larger selection of columns and analysis conditions such as packed and capillary columns as well as a Thermal Conductivity Detector in addition to the Flame Ionization Detector. Analysis times range from 14 min to 60 min.  
1.1.2 Procedure B (Sections 15 – 23)—Is restricted to only 3 capillary columns and requires no sample dilution. In addition, Procedure B is used not only for the sample types described in Procedure A but also for the analysis of samples containing biodiesel mixtures B5, B10, and B20. The analysis time, when using Procedure B (Accelerated D2887), is reduced to about 8 min.  
1.2 This test method is not to be used for the analysis of gasoline samples or gasoline components. These types of samples must be analyzed by Test Method D7096.  
1.3 The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for information only and are not considered 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: 30-Jun-2023
• ICS: 75.080 - Petroleum products in general
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.04.0H - Chromatographic Distribution Methods

Relations

• Replaces: ASTM D2887-22e1 - Standard Test Method for Boiling Range Distribution of Petroleum Fractions by Gas Chromatography
• Effective Date: 01-Jul-2023
• Refers: ASTM D6300-24 - Standard Practice for Determination of Precision and Bias Data for Use in Test Methods for Petroleum Products, Liquid Fuels, and Lubricants
• Effective Date: 01-Mar-2024
• Refers: ASTM D6708-24 - Standard Practice for Statistical Assessment and Improvement of Expected Agreement Between Two Test Methods that Purport to Measure the Same Property of a Material
• Effective Date: 01-Mar-2024
• Refers: ASTM D4175-23a - Standard Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants
• Effective Date: 15-Dec-2023
• Refers: ASTM D6300-23a - Standard Practice for Determination of Precision and Bias Data for Use in Test Methods for Petroleum Products, Liquid Fuels, and Lubricants
• Effective Date: 01-Dec-2023
• Refers: ASTM D86-23ae1 - Standard Test Method for Distillation of Petroleum Products and Liquid Fuels at Atmospheric Pressure
• Effective Date: 01-Dec-2023
• Refers: ASTM D86-23a - Standard Test Method for Distillation of Petroleum Products and Liquid Fuels at Atmospheric Pressure
• Effective Date: 01-Dec-2023
• Refers: ASTM D6299-23a - Standard Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measurement System Performance
• Effective Date: 01-Dec-2023
• Refers: ASTM D6299-23e1 - Standard Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measurement System Performance
• Effective Date: 01-Jul-2023
• Refers: ASTM D6300-23 - Standard Practice for Determination of Precision and Bias Data for Use in Test Methods for Petroleum Products, Liquid Fuels, and Lubricants
• Effective Date: 01-Jul-2023
• Refers: ASTM D4175-23e1 - Standard Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants
• Effective Date: 01-Jul-2023
• Refers: ASTM D86-23 - Standard Test Method for Distillation of Petroleum Products and Liquid Fuels at Atmospheric Pressure
• Effective Date: 01-Mar-2023
• Refers: ASTM D6708-21 - Standard Practice for Statistical Assessment and Improvement of Expected Agreement Between Two Test Methods that Purport to Measure the Same Property of a Material
• Effective Date: 01-May-2021
• Referred By: ASTM D6743-20 - Standard Test Method for Thermal Stability of Organic Heat Transfer Fluids
• Effective Date: 01-Jul-2023
• Referred By: ASTM D7863-22 - Standard Guide for Evaluation of Convective Heat Transfer Coefficient of Liquids
• Effective Date: 01-Jul-2023

Overview

ASTM D2887-23, titled Standard Test Method for Boiling Range Distribution of Petroleum Fractions by Gas Chromatography, is an established ASTM International standard that specifies methods for determining the boiling range distribution of petroleum products and fractions. This standard is applicable to samples with a final boiling point of 538 °C (1000 °F) or lower at atmospheric pressure and with a boiling range greater than 55.5 °C (100 °F). It provides a gas chromatographic alternative to traditional distillation techniques, offering reliable results for quality control, product specification, and process monitoring within petroleum refining and related industries.

Key Topics

• Scope and Applicability: ASTM D2887-23 is suitable for the analysis of petroleum fractions, including biodiesel blends, but excludes gasoline samples or components.
• Test Methods:
  • Procedure A permits the use of various columns and detectors, including packed and capillary columns, with flame ionization or thermal conductivity detection. Analysis times typically range from 14 to 60 minutes.
  • Procedure B, designed for accelerated testing, restricts analysis to three capillary columns, eliminates the need for sample dilution, and includes specific provisions for biodiesel (FAME) mixtures such as B5, B10, and B20. Procedure B reduces analysis time to about 8 minutes.
• Equivalency: Boiling range distributions from this gas chromatographic method are essentially equivalent to true boiling point (TBP) distillation (see ASTM D2892), but not directly comparable to low-efficiency methods like ASTM D86 or D1160.
• Significance: This method provides critical insights into the composition of petroleum feedstocks and products, supporting process optimization, regulatory compliance, and product quality assurance.

Applications

ASTM D2887-23 is widely used in the following areas:

• Petroleum Refining: Monitoring and control of refining operations, where boiling range distribution informs decision-making and process adjustments.
• Product Specification Testing: Ensures compliance with internal and regulatory product specifications; can be used as an alternative or supplement to distillation-based methods when agreed upon by involved parties.
• Blend Analysis: Particularly beneficial for rapid analysis of biodiesel blends, including FAME esters mixed with ultra-low sulfur diesel, supporting both product development and quality control.
• Research and Development: Assists in the evaluation of new feedstocks, refining processes, and fuel formulations.
• Analytical Laboratories: Provides a standardized method for characterizing petroleum fractions, aiding in routine testing and inter-laboratory comparisons.

Related Standards

Several other ASTM methods and standards are closely related and often referenced alongside ASTM D2887-23:

• ASTM D2892: Standard Test Method for Distillation of Crude Petroleum (15-Theoretical Plate Column), the reference method for true boiling point distillation.
• ASTM D7096: Test Method specifically designated for gasoline boiling range analysis by wide-bore capillary gas chromatography.
• ASTM D86 / ASTM D1160: Methods for atmospheric and reduced-pressure distillation of petroleum products, respectively.
• ASTM D4057: Practice for Manual Sampling of Petroleum and Petroleum Products.
• ASTM D6708, D6299, D4626: Practices covering statistical quality assurance and calibration relevant to gas chromatographic methods.

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Keywords: ASTM D2887-23, boiling range distribution, gas chromatography, petroleum fractions, petroleum refining, TBP distillation, product specification, biodiesel blends, process control, ASTM standards.

Standards Content (Sample)

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: D2887 − 23
Standard Test Method for
Boiling Range Distribution of Petroleum Fractions by Gas
Chromatography
This standard is issued under the fixed designation D2887; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope* priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
1.1 This test method covers the determination of the boiling
1.5 This international standard was developed in accor-
range distribution of petroleum products. The test method is
dance with internationally recognized principles on standard-
applicable to petroleum products and fractions having a final
ization established in the Decision on Principles for the
boiling point of 538 °C (1000 °F) or lower at atmospheric
Development of International Standards, Guides and Recom-
pressure as measured by this test method. This test method is
mendations issued by the World Trade Organization Technical
limited to samples having a boiling range greater than 55.5 °C
Barriers to Trade (TBT) Committee.
(100 °F), and having a vapor pressure sufficiently low to permit
sampling at ambient temperature.
2. Referenced Documents
NOTE 1—Since a boiling range is the difference between two
2.1 ASTM Standards:
temperatures, only the constant of 1.8 °F ⁄°C is used in the conversion of
D86 Test Method for Distillation of Petroleum Products and
the temperature range from one system of units to another.
Liquid Fuels at Atmospheric Pressure
1.1.1 Procedure A (Sections 6 – 14)—Allows a larger
D1160 Test Method for Distillation of Petroleum Products at
selection of columns and analysis conditions such as packed
Reduced Pressure
and capillary columns as well as a Thermal Conductivity
D2892 Test Method for Distillation of Crude Petroleum
Detector in addition to the Flame Ionization Detector. Analysis
(15-Theoretical Plate Column)
times range from 14 min to 60 min.
D4057 Practice for Manual Sampling of Petroleum and
1.1.2 Procedure B (Sections 15 – 23)—Is restricted to only
Petroleum Products
3 capillary columns and requires no sample dilution. In
D4175 Terminology Relating to Petroleum Products, Liquid
addition, Procedure B is used not only for the sample types
Fuels, and Lubricants
described in Procedure A but also for the analysis of samples
D4626 Practice for Calculation of Gas Chromatographic
containing biodiesel mixtures B5, B10, and B20. The analysis
Response Factors
time, when using Procedure B (Accelerated D2887), is reduced
D6299 Practice for Applying Statistical Quality Assurance
to about 8 min.
and Control Charting Techniques to Evaluate Analytical
1.2 This test method is not to be used for the analysis of
Measurement System Performance
gasoline samples or gasoline components. These types of
D6300 Practice for Determination of Precision and Bias
samples must be analyzed by Test Method D7096.
Data for Use in Test Methods for Petroleum Products,
Liquid Fuels, and Lubricants
1.3 The values stated in SI units are to be regarded as
D6708 Practice for Statistical Assessment and Improvement
standard. The values given in parentheses after SI units are
of Expected Agreement Between Two Test Methods that
provided for information only and are not considered standard.
Purport to Measure the Same Property of a Material
1.4 This standard does not purport to address all of the
D7096 Test Method for Determination of the Boiling Range
safety concerns, if any, associated with its use. It is the
Distribution of Gasoline by Wide-Bore Capillary Gas
responsibility of the user of this standard to establish appro-
Chromatography
D7169 Test Method for Boiling Point Distribution of
This test method is under the jurisdiction of Committee D02 on Petroleum
Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcom-
mittee D02.04.0H on Chromatographic Distribution Methods. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved July 1, 2023. Published December 2023. Originally contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
ɛ1
approved in 1973. Last previous edition approved in 2022 as D2887 – 22 . DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D2887-23. the ASTM website.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D2887 − 23
Samples with Residues Such as Crude Oils and Atmo- subscripted suffix denotes the number of carbon atoms (for
spheric and Vacuum Residues by High Temperature Gas example, normal decane = n-C ; isotetradecane = i-C ).
10 14
Chromatography
4. Summary of Test Method
E29 Practice for Using Significant Digits in Test Data to
Determine Conformance with Specifications
4.1 The boiling range distribution determination by distilla-
E260 Practice for Packed Column Gas Chromatography
tion is simulated by the use of gas chromatography. A nonpolar
E355 Practice for Gas Chromatography Terms and Relation-
packed or open tubular (capillary) gas chromatographic col-
ships
umn is used to elute the hydrocarbon components of the sample
E516 Practice for Testing Thermal Conductivity Detectors
in order of increasing boiling point. The column temperature is
Used in Gas Chromatography
raised at a reproducible linear rate and the area under the
E594 Practice for Testing Flame Ionization Detectors Used
chromatogram is recorded throughout the analysis. Boiling
in Gas or Supercritical Fluid Chromatography
points are assigned to the time axis from a calibration curve
obtained under the same chromatographic conditions by ana-
3. Terminology
lyzing a known mixture of hydrocarbons covering the boiling
range expected in the sample. From these data, the boiling
3.1 Definitions—This test method makes reference to many
common gas chromatographic procedures, terms, and relation- range distribution can be obtained.
ships. Detailed definitions of these can be found in Practices
4.2 Procedure A and Procedure B yield essentially the same
E260, E355, and E594.
results. See Sections 14 and 23, and the accompanying research
reports.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 area slice, n—the area, resulting from the integration
5. Significance and Use
of the chromatographic detector signal, within a specified
retention time interval. In area slice mode (see 6.3.2), peak
5.1 The boiling range distribution of petroleum fractions
detection parameters are bypassed and the detector signal
provides an insight into the composition of feedstocks and
integral is recorded as area slices of consecutive, fixed duration
products related to petroleum refining processes. The gas
time intervals.
chromatographic simulation of this determination can be used
3.2.2 corrected area slice, n—an area slice corrected for to replace conventional distillation methods for control of
baseline offset, by subtraction of the exactly corresponding refining operations. This test method can be used for product
area slice in a previously recorded blank (non-sample) analy- specification testing with the mutual agreement of interested
sis. parties.
3.2.3 cumulative corrected area, n—the accumulated sum of 5.2 Boiling range distributions obtained by this test method
corrected area slices from the beginning of the analysis through
are essentially equivalent to those obtained by true boiling
a given retention time, ignoring any non-sample area (for point (TBP) distillation (see Test Method D2892). They are not
example, solvent).
equivalent to results from low efficiency distillations such as
those obtained with Test Method D86 or D1160.
3.2.4 final boiling point (FBP), n—the temperature (corre-
sponding to the retention time) at which a cumulative corrected
5.3 Procedure B was tested with biodiesel mixtures and
area count equal to 99.5 % of the total sample area under the
reports the Boiling Point Distribution of FAME esters of
chromatogram is obtained.
vegetable and animal origin mixed with ultra low sulfur diesel.
3.2.5 initial boiling point (IBP), n—the temperature (corre-
Procedure A
sponding to the retention time) at which a cumulative corrected
area count equal to 0.5 % of the total sample area under the
6. Apparatus
chromatogram is obtained.
6.1 Chromatograph—The gas chromatograph used must
3.2.6 slice rate, n—the time interval used to integrate the
have the following performance characteristics:
continuous (analog) chromatographic detector response during
6.1.1 Detector—Either a flame ionization or a thermal
an analysis. The slice rate is expressed in hertz (for example,
conductivity detector may be used. The detector must have
integrations or slices per second).
sufficient sensitivity to detect 1.0 % dodecane with a peak
3.2.7 slice time, n—the time associated with the end of each
height of at least 10 % of full scale on the recorder under
contiguous area slice. The slice time is equal to the slice
conditions prescribed in this test method and without loss of
number divided by the slice rate.
resolution as defined in 9.3.1. When operating at this sensitiv-
3.2.8 total sample area, n—the cumulative corrected area,
ity level, detector stability must be such that a baseline drift of
from the initial area point to the final area point, where the
not more than 1 % of full scale per hour is obtained. The
chromatographic signal is considered to have returned to
detector must be capable of operating continuously at a
baseline after complete sample elution.
temperature equivalent to the maximum column temperature
employed. Connection of the column to the detector must be
3.3 Abbreviations:
such that no temperature below the column temperature exists.
3.3.1 A common abbreviation of hydrocarbon compounds is
to designate the number of carbon atoms in the compound. A
NOTE 2—It is not desirable to operate a thermal conductivity detector at
prefix is used to indicate the carbon chain form, while a a temperature higher than the maximum column temperature employed.
D2887 − 23
Operation at higher temperature generally contributes to higher noise
columns, inlet pressures from 10 kPa to 70 kPa (1.5 psig to
levels and greater drift and can shorten the useful life of the detector.
10 psig) have been found to be suitable.
6.1.2 Column Temperature Programmer—The chromato-
6.1.6 Microsyringe—A microsyringe is needed for sample
graph must be capable of linear programmed temperature
introduction.
operation over a range sufficient to establish a retention time of
NOTE 3—Automatic sampling devices or other sampling means, such as
at least 1 min for the IBP and to elute compounds up to a
indium encapsulation, can be used provided: the system can be operated
boiling temperature of 538 °C (1000 °F) before reaching the
at a temperature sufficiently high to completely vaporize hydrocarbons
upper end of the temperature program. The programming rate
with atmospheric boiling points of 538 °C (1000 °F), and the sampling
must be sufficiently reproducible to obtain retention time system is connected to the chromatographic column avoiding any cold
temperature zones.
repeatability of 0.1 min (6 s) for each component in the
calibration mixture described in 7.8.
6.2 Column—Any column and conditions may be used that
6.1.3 Cryogenic Column Cooling—Column starting tem-
provide separation of typical petroleum hydrocarbons in order
peratures below ambient will be required if samples with IBPs
of increasing boiling point and meet the column performance
of less than 93 °C (200 °F) are to be analyzed. This is typically
requirements of 9.3.1 and 9.3.3. Successfully used columns
provided by adding a source of either liquid carbon dioxide or
and conditions are given in Table 1.
liquid nitrogen, controlled through the oven temperature cir-
6.3 Data Acquisition System:
cuitry. Excessively low initial column temperature must be
6.3.1 Recorder—A 0 mV to 1 mV range recording potenti-
avoided to ensure that the stationary phase remains liquid. The
ometer or equivalent, with a full-scale response time of 2 s or
initial temperature of the column should be only low enough to
less may be used.
obtain a calibration curve meeting the specifications of the
6.3.2 Integrator—Means must be provided for determining
method.
the accumulated area under the chromatogram. This can be
6.1.4 Sample Inlet System—The sample inlet system must
done by means of an electronic integrator or computer-based
be capable of operating continuously at a temperature equiva-
chromatography data system. The integrator/computer system
lent to the maximum column temperature employed, or provide
must have normal chromatographic software for measuring the
for on-column injection with some means of programming the
retention time and areas of eluting peaks (peak detection
entire column, including the point of sample introduction, up to
mode). In addition, the system must be capable of converting
the maximum temperature required. Connection of the column
the continuously integrated detector signal into area slices of
to the sample inlet system must be such that no temperature
fixed duration. These contiguous area slices, collected for the
below the column temperature exists.
entire analysis, are stored for later processing. The electronic
6.1.5 Flow Controllers—The gas chromatograph must be
range of the integrator/computer (for example, 1 V, 10 V) must
equipped with mass flow controllers capable of maintaining
be within the linear range of the detector/electrometer system
carrier gas flow constant to 61 % over the full operating
used. The system must be capable of subtracting the area slice
temperature range of the column. The inlet pressure of the
of a blank run from the corresponding area slice of a sample
carrier gas supplied to the gas chromatograph must be suffi-
run.
ciently high to compensate for the increase in column back-
pressure as the column temperature is raised. An inlet pressure
NOTE 4—Some gas chromatographs have an algorithm built into their
of 550 kPa (80 psig) has been found satisfactory with the
operating software that allows a mathematical model of the baseline
packed columns described in Table 1. For open tubular profile to be stored in memory. This profile is automatically subtracted
TABLE 1 Typical Operating Conditions for Procedure A
Packed Columns 1 2 3 4 Open Tubular Columns 5 6
Column length, m (ft) 1.2 (4) 1.5 (5) 0.5 (1.5) 0.6 (2) Column length (m) 5 10
Column outside diameter, mm 6.4 (1/4) 3.2 (1/8) 3.2 (1/8) 6.4 (1/8) Column inner diameter (mm) 0.53 0.53
(in.)
Liquid phase OV-1 SE-30 UC-W98 SE-30 Stationary phase HP-1 HP-1
Percent liquid phase 3 5 10 10 Stationary phase thickness 0.88 2.65
(μm)
A B C C
Support material S G P P Carrier gas helium helium
Support mesh size 60/80 60/80 80/100 60/80 Carrier gas flow rate, mL/min 12 12
Initial column temperature, °C –20 –40 –30 –50 Initial column temperature, °C 35 35
Final column temperature, °C 360 350 360 390 Final column temperature, °C 350 350
Programming rate, °C/min 10 6.5 10 7.5 Programming rate, °C/min 10 20
Carrier gas helium helium N helium Detector FID FID
Carrier gas flow, mL/min 40 30 25 60 Detector temperature, °C 380 370
Detector TC FID FID TC Injector temperature, °C cool on-column cool on-column
Detector temperature, °C 360 370 360 390 Sample size, μL 1 0.1–0.2
Injection port temperature, °C 360 370 350 390 Sample concentration mass % 2 neat
Sample size, μ 4 0.3 1 5
A
Diatoport S; silane treated.
B
Chromosorb G (AW-DMS).
C
Chromosorb P, acid washed.
D2887 − 23
from the detector signal on subsequent sample analyses to compensate for
7.8 Calibration Mixture—An accurately weighed mixture of
any baseline offset. Some integration systems also store and automatically
approximately equal mass quantities of n-hydrocarbons dis-
subtract a blank analysis from subsequent analytical determinations.
solved in carbon disulfide (CS ). (Warning—Carbon disulfide
is extremely volatile, flammable, and toxic.) The mixture shall
7. Reagents and Materials
cover the boiling range from n-C to n-C , but does not need
5 44
7.1 Purity of Reagents—Reagent grade chemicals shall be
to include every carbon number (see Note 5).
used in all tests. Unless otherwise indicated, it is intended that
7.8.1 At least one compound in the mixture must have a
all reagents conform to the specifications of the Committee on
boiling point lower than the IBP of the sample and at least one
Analytical Reagents of the American Chemical Society where
compound in the mixture must have a boiling point higher than
such specifications are available. Other grades may be used,
the FBP of the sample. Boiling points of n-paraffins are listed
provided it is first ascertained that the reagent is of sufficiently
in Table 2.
high purity to permit its use without lessening the accuracy of
7.8.1.1 If necessary, for the calibration mixture to have a
the determination.
compound with a boiling point below the IBP of the sample,
7.2 Liquid Phase for Columns—Methyl silicone gums and
propane or butane can be added to the calibration mixture,
liquids provide the proper chromatographic hydrocarbon elu-
non-quantitatively, by bubbling the gaseous compound into the
tion characteristics for this test method.
calibration mixture in a septum sealed vial using a gas syringe.
7.3 Solid Support for Packed Columns—Chromatographic
NOTE 5—Calibration mixtures containing normal paraffins with the
grade diatomateous earth solid support material within a carbon numbers 5, 6, 7, 8, 9, 10, 11, 12, 14, 15, 16, 17, 18, 20, 24, 28, 32,
36, 40, and 44 have been found to provide a sufficient number of points to
particle size range from 60 to 100 sieve mesh size is recom-
generate a reliable calibration curve.
mended.
7.8.2 Packed Columns—The final concentration should be
7.4 Carrier Gas—Helium or nitrogen of high purity
approximately ten parts of the n-paraffin mixture to one
(99.999 % pure). (Warning—Helium and nitrogen are com-
hundred parts of CS .
pressed gases under high pressure.) Additional purification is
recommended by the use of molecular sieves or other suitable
agents to remove water, oxygen, and hydrocarbons. The use of
A, B, C
TABLE 2 Boiling Points of Normal Paraffins
helium and nitrogen as carrier gas have valid precision
Carbon Boiling Boiling Carbon Boiling Boiling
statements. The precision for using nitrogen as carrier gas is
Number Point, °C Point, °F Number Point, °C Point, °F
described in Annex A2. Available pressure must be sufficient to
1 –162 –259 23 380 716
ensure a constant carrier gas flow rate (see 6.1.5). Appendix X5 2 –89 –127 24 391 736
3 –42 –44 25 402 755
lists conditions for using hydrogen as carrier gas for Procedure
4 0 31 26 412 774
A. Note X5.1 also states that results with alternative carriers
5 36 97 27 422 791
6 69 156 28 431 808
are not considered to be valid D2887 Procedure A results until
7 98 209 29 440 825
a valid precision (r and R) statement is obtaind from an ILS
8 126 258 30 449 840
using Procedure A.
9 151 303 31 458 856
10 174 345 32 466 870
7.5 Hydrogen—Hydrogen of high purity (99.999 % pure) is
11 196 385 33 474 885
used as fuel for the flame ionization detector (FID).
12 216 421 34 481 898
13 235 456 35 489 912
(Warning—Hydrogen is an extremely flammable gas under
14 254 488 36 496 925
high pressure.)
15 271 519 37 503 937
16 287 548 38 509 948
7.6 Air—High purity (for example, hydrocarbon free) com-
17 302 576 39 516 961
pressed air is used as the oxidant for the flame ionization
18 316 601 40 522 972
19 330 626 41 528 982
detector (FID). (Warning—Compressed air is a gas under high
20 344 651 42 534 993
pressure and supports combustion.)
21 356 674 43 540 1004
22 369 695 44 545 1013
7.7 Column Resolution Test Mixture—For packed columns,
A
API Project 44, October 31, 1972 is believed to have provided the original normal
a nominal mixture of 1 % by mass each of n-C and n-C
16 18
paraffin boiling point data that are listed in Table 2. However, over the years some
paraffin in a suitable solvent, such as n-octane, for use in
of the data contained in both API Project 44 (Thermodynamics Research Center
testing the column resolution. (Warning—n-octane is flam-
Hydrocarbon Project) and Test Method D2887 have changed, and they are no
longer equivalent. Table 2 represents the current normal paraffin boiling point
mable and harmful if inhaled.) The calibration mixture speci-
values accepted by Subcommittee D02.04 and found in all test methods under the
fied in 7.8.2 may be used as a suitable alternative, provided the
jurisdiction of Section D02.04.0H.
B
concentrations of the n-C and n-C components are nomi-
Test Method D2887 has traditionally used n-paraffin boiling points rounded to the
16 18
nearest whole degree for calibration. The boiling points listed in Table 2 are correct
nally 1.0 % by mass each. For open tubular columns, use the
to the nearest whole number in both degrees Celsius and degrees Fahrenheit.
mixture specified in 7.8.3.
However, if a conversion is made from one unit to the other and then rounded to
a whole number, the result will not agree with the table value for a few carbon
numbers. For example, the boiling point of n-heptane is 98.425 °C, which is
ACS Reagent Chemicals, Specifications and Procedures for Reagents and
correctly rounded to 98 °C in the table. However, converting 98.425 °C gives
Standard-Grade Reference Materials, American Chemical Society, Washington,
209.165 °F, which rounds to 209 °F, while converting 98 °C gives 208.4 °F, which
DC. For suggestions on the testing of reagents not listed by the American Chemical
rounds to 208 °F. Carbon numbers 2, 4, 7, 8, 9, 13, 14, 15, 16, 25, 27, and 32 are
Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset,
affected by rounding.
C
U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharma-
Table X6.1 lists the current boiling points of n-paraffins approved by API.
copeial Convention, Inc. (USPC), Rockville, MD.
D2887 − 23
7.8.3 Open Tubular Columns—The final concentration 9. Preparation of Apparatus
should be approximately one part of the n-paraffin mixture to
9.1 Chromatograph—Place in service in accordance with
one hundred parts of CS .
the manufacturer’s instructions. Typical operating conditions
7.9 Reference Gas Oil (Tables 3 and 4)—A reference mate-
are shown in Table 1.
rial that has been analyzed by laboratories participating in the
9.1.1 When a FID is used, regularly remove the deposits
test method cooperative study. Accepted Reference Values
formed in the detector from combustion of the silicone liquid
(ARV) for the boiling range distribution of these reference oils
phase decomposition products. These deposits will change the
are given in Tables 3 and 4. Addition of new reference material
response characteristics of the detector.
to this standard requires the ARV of the new reference material
9.1.2 If the sample inlet system is heated above 300 °C
to be determined in accordance with a similar cooperative
(572 °F), a blank analysis must be made after a new septum is
study using a minimum participation of 16 laboratories as
installed to ensure that no extraneous detector response is
described in Practice D6299 (6.2.2.1) for determination of
produced by septum bleed. At the sensitivity levels commonly
check standard ARV using interlaboratory testing. Results for
employed in this test method, conditioning of the septum at the
the new reference material provided by each laboratory shall be
operating temperature of the sample inlet system for several
validated by an accompanying qualifying result using a current
hours will minimize this problem. A recommended practice is
reference oil in this standard.
to change the septum at the end of a series of analyses rather
8. Sampling than at the beginning of the series.
8.1 Samples to be analyzed by this test method must be
9.2 Column Preparation:
obtained using the procedures outlined in Practice D4057.
9.2.1 Packed Columns—Any satisfactory method that will
8.2 The test specimen to be analyzed must be homogeneous produce a column meeting the requirements of 9.3.1 and 9.3.3
and free of dust or undissolved material. can be used. In general, use liquid phase loadings of 3 % to
A, B
TABLE 3 Test Method D2887 Reference Gas Oil No. 1
ARV RGO No. 1 Batch 1 ARV RGO No. 1 Batch 2 ARV RGO No. 1 Batch 3
Mid- Allowed Mid- Allowed Mid- Allowed
% OFF Lower Upper point Devia- Lower Upper point Devia- Lower Upper point Devia- % OFF
Limit Limit Value tion Limit Limit Value tion Limit Limit Value tion
(°F) (°F) (°F) (°F) (°F) (°F) (°F) (°F) (°F) (°F) (°F) (°F)
IBP 224.4 251.6 238.0 13.6 225.8 253.2 239.5 13.7 224.2 251.4 237.8 13.6 IBP
5 282.4 295.6 289.0 6.6 297.4 311.0 304.2 6.8 296.8 310.4 303.6 6.8 5
10 328.7 343.3 336.0 7.3 341.2 356.0 348.6 7.4 338.8 353.6 346.2 7.4 10
20 420.3 437.7 429.0 8.7 426.0 443.4 434.7 8.7 431.4 449.0 440.2 8.8 20
30 487.6 504.4 496.0 8.4 490.2 507.0 498.6 8.4 502.4 519.5 510.9 8.6 30
40 540.3 555.7 548.0 7.7 544.4 559.8 552.1 7.7 554.8 570.2 562.5 7.7 40
50 586.3 601.7 594.0 7.7 586.1 601.5 593.8 7.7 593.2 608.6 600.9 7.7 50
60 621.3 636.7 629.0 7.7 621.3 636.7 629.0 7.7 628.5 643.9 636.2 7.7 60
70 661.3 676.7 669.0 7.7 661.0 676.4 668.7 7.7 667.3 682.7 675.0 7.7 70
80 701.3 716.7 709.0 7.7 704.5 719.9 712.2 7.7 713.0 728.4 720.7 7.7 80
90 751.3 766.7 759.0 7.7 756.6 772.0 764.3 7.7 764.9 780.3 772.6 7.7 90
95 788.0 806.0 797.0 9.0 794.0 812.0 803.0 9.0 799.5 817.5 808.5 9.0 95
FBP 865.8 908.2 887.0 21.2 866.1 908.5 887.3 21.2 853.5 895.9 874.7 21.2 FBP
ARV RGO No. 1 Batch 1 ARV RGO No. 1 Batch 2 ARV RGO No. 1 Batch 3
Mid- Allowed Mid- Allowed Mid- Allowed
% OFF Lower Upper point Devia- Lower Upper point Devia- Lower Upper point Devia- % OFF
Limit Limit Value tion Limit Limit Value tion Limit Limit Value tion
(°C) (°C) (°C) (°C) (°C) (°C) (°C) (°C) (°C) (°C) (°C) (°C)
IBP 106.9 122.0 114.4 7.6 107.7 122.9 115.3 7.6 106.8 121.9 114.3 7.5 IBP
5 139.1 146.4 142.8 3.6 147.5 155.0 151.2 3.8 147.1 154.6 150.9 3.8 5
10 164.9 172.9 168.9 4.0 171.8 180.0 175.9 4.1 170.4 178.7 174.6 4.1 10
20 215.7 225.4 220.6 4.8 218.9 228.6 223.7 4.9 221.9 231.7 226.8 4.9 20
30 253.1 262.4 257.8 4.7 254.6 263.9 259.2 4.7 261.3 270.8 266.1 4.8 30
40 282.4 290.9 286.7 4.3 284.7 293.2 288.9 4.3 290.4 299.0 294.7 4.3 40
50 307.9 316.5 312.2 4.3 307.8 316.4 312.1 4.3 311.8 320.3 316.0 4.3 50
60 327.4 335.9 331.7 4.3 327.4 335.9 331.7 4.3 331.4 340.0 335.7 4.3 60
70 349.6 358.2 353.9 4.3 349.4 358.0 353.7 4.3 353.0 361.5 357.2 4.3 70
80 371.8 380.4 376.1 4.3 373.6 382.2 377.9 4.3 378.3 386.9 382.6 4.3 80
90 399.6 408.2 403.9 4.3 402.6 411.1 406.8 4.3 407.2 415.7 411.4 4.3 90
95 420.0 430.0 425.0 5.0 423.3 433.3 428.3 5.0 426.4 436.4 431.4 5.0 95
FBP 463.2 486.8 475.0 11.8 463.4 486.9 475.2 11.8 456.4 480.0 468.2 11.8 FBP
A
Consensus results for Batch 2 obtained from 30 laboratories in 1995 (supporting data have been filed at ASTM International Headquarters and may be obtained by
requesting Research Report RR:D02-1407. Contact ASTM Customer Service at [e-mail].).
B
Supporting data for Batch 3 have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:D02-1913. Contact ASTM
Customer Service at [e-mail].
D2887 − 23
A
TABLE 4 Test Method D2887 Reference Gas Oil No. 2
ARV RGO No. 2 ARV RGO No. 2
Allowed Allowed
% OFF % OFF
Lower Limit Upper Limit Midpoint Value Deviation Lower Limit Upper Limit Midpoint Value Deviation
(°F) (°F) (°F) (°F) (°C) (°C) (°C) (°C)
IBP 209.6 234.7 222.2 12.6 98.7 112.6 105.7 7.0 IBP
5 335.1 349.8 342.5 7.4 168.4 176.6 172.5 4.1 5
10 376.3 392.2 384.2 8.0 191.3 200.1 195.7 4.4 10
20 442.7 460.7 451.7 9.0 228.2 238.2 233.2 5.0 20
30 503.4 520.6 512.0 8.6 261.9 271.4 266.7 4.8 30
40 559.9 575.3 567.6 7.7 293.3 301.9 297.6 4.3 40
50 601.6 617.0 609.3 7.7 316.4 325.0 320.7 4.3 50
60 638.8 654.2 646.5 7.7 337.1 345.6 341.4 4.3 60
70 669.4 684.8 677.1 7.7 354.1 362.7 358.4 4.3 70
80 704.3 719.7 712.0 7.7 373.5 382.0 377.8 4.3 80
90 755.3 770.7 763.0 7.7 401.9 410.4 406.1 4.3 90
95 799.0 817.0 808.0 9.0 426.1 436.1 431.1 5.0 95
FBP 905.3 947.7 926.5 21.2 485.2 508.7 496.9 11.8 FBP
A
Consensus results for Reference Gas Oil No. 2 obtained from 32 laboratories in 2009.
10 %. Condition the column at the maximum operating tem- set the column and detector gas flows. Before heating the
perature to reduce baseline shifts due to bleeding of the column column, allow the system to purge with carrier gas at ambient
substrate. The column can be conditioned very rapidly and temperature for at least 30 min.
effectively using the following procedure:
9.2.2.2 Increase the oven temperature about 5 °C to 10 °C
9.2.1.1 Connect the column to the inlet but leave the
per minute to the final operating temperature and hold for about
detector end free.
30 min.
9.2.1.2 Purge the column thoroughly at ambient temperature
9.2.2.3 Cycle the gas chromatograph several times through
with carrier gas.
its temperature program until a stable baseline is obtained.
9.2.1.3 Turn off the carrier gas and allow the column to
9.3 System Performance Specification:
depressurize completely.
9.3.1 Column Resolution—The column resolution, influ-
9.2.1.4 Seal off the open end (detector) of the column with
enced by both the column physical parameters and operating
an appropriate fitting.
conditions, affects the overall determination of boiling range
9.2.1.5 Raise the column temperature to the maximum
distribution. Resolution is therefore specified to maintain
operating temperature.
equivalence between different systems (laboratories) employ-
9.2.1.6 Hold the column at this temperature for at least 1 h
ing this test method. Resolution is determined using Eq 1 and
with no flow through the column.
the C and C paraffins from a column resolution test mixture
9.2.1.7 Cool the column to ambient temperature. 16 18
analysis (see 7.7 and Section 10), and is illustrated in Fig. 1.
9.2.1.8 Remove the cap from the detector end of the column
Resolution (R) should be at least three, using the identical
and turn the carrier gas back on.
conditions employed for sample analyses:
9.2.1.9 Program the column temperature up to the maxi-
mum several times with normal carrier gas flow. Connect the
R 5 2 t 2 t / 1.699 w 1w (1)
~ ! @ ~ !#
2 1 2 1
free end of the column to the detector.
where:
9.2.1.10 An alternative method of column conditioning that
R = resolution,
has been found effective for columns with an initial loading of
t = time(s) for the n-C peak maximum,
1 16
10 % liquid phase consists of purging the column with carrier
t = time(s) for the n-C peak maximum,
2 18
gas at the normal flow rate while holding the column at the
w = peak width(s), at half height, of the n-C peak, and
1 16
maximum operating temperature for 12 h to 16 h, while de-
w = peak width(s), at half height, of the n-C peak.
2 18
tached from the detector.
9.2.2 Open Tubular Columns—Open tubular columns with 9.3.2 Detector Response Calibration—This test method as-
cross-linked and bonded stationary phases are available from sumes that the detector response to petroleum hydrocarbons is
many manufacturers and are usually pre-conditioned. These proportional to the mass of individual components. This must
columns have much lower column bleed than packed columns. be verified when the system is put in service, and whenever any
Column conditioning is less critical with these columns but changes are made to the system or operational parameters.
some conditioning may be necessary. The column can be Analyze the calibration mixture using the identical procedure
conditioned very rapidly and effectively using the following to be used for the analysis of samples (see Section 10).
procedure. Calculate the relative response factor for each n-paraffin
9.2.2.1 Once the open tubular column has been properly (relative to n-decane) in accordance with Practice D4626 and
installed into the gas chromatograph and tested to be leak free, Eq 2:
D2887 − 23
FIG. 1 Column Resolution Parameters
F 5 ~M /A !/~M /A ! (2) use the area slice mode of integration. The recommended slice
n n n 10 10
rate for this test method is given in 12.1.2. Other slice rates
where:
may be used if within the limits of 0.02 % and 0.2 % of the
F = relative response factor,
n
retention time of the final calibration component (C ). Larger
M = mass of the n-paraffin in the mixture,
n
slice rates may be used, as may be required for other reasons,
A = peak area of the n-paraffin in the mixture,
n
if provision is made to accumulate (bunch) the slice data to
M = mass of the n-decane in the mixture, and
within these limits prior to determination of the boiling range
A = peak area of the n-decane in the mixture.
distribution.
The relative response factor (F ) of each n-paraffin must not
n
10.1.3 At the exact time set by the schedule, inject either the
deviate from unity (1) by more than 610 %.
calibration mixture or sample into the chromatograph; or make
9.3.3 Column Elution Characteristics—The column
no injection (baseline blank). At the time of injection, start the
material, stationary phase, or other parameters can affect the
chromatograph time cycle and the integrator/computer data
elution order of non-paraffinic sample components, resulting in
acquisition. Follow the analysis sequence protocol for all
deviations from a TBP versus retention time relationship. If
subsequent repetitive analyses or calibrations. Since complete
stationary phases other than those referenced in 7.3 are used,
resolution of sample peaks is not expected, do not change the
the retention times of a few alkylbenzenes (for example,
detector sensitivity setting during the analysis.
o-xylene, n-butyl-benzene, 1,3,5-triisopropylbenzene, n-decyl-
10.2 Baseline Compensation Analysis—A baseline compen-
benzene, and tetradecylbenzene) across the boiling range
sation analysis, or baseline blank, is performed exactly like an
should be analyzed to make certain that the column is
analysis except no injection is made. A blank analysis must be
separating in accordance with the boiling point order (see
performed at least once per day. The blank analysis is neces-
Appendix X1).
sary due to the usual occurrence of chromatographic baseline
instability and is subtracted from sample analyses to remove
10. Calibration and Standardization
any non-sample slice area from the chromatographic data. The
10.1 Analysis Sequence Protocol—Define and use a prede-
blank analysis is typically performed prior to sample analyses,
termined schedule of analysis events designed to achieve
but may be useful if determined between samples or at the end
maximum reproducibility for these determinations. The sched-
of a sample sequence to provide additional data regarding
ule will include cooling the column oven to the initial starting
instrument operation or residual sample carryover from previ-
temperature, equilibration time, sample injection and system
ous sample analyses. Attention must be given to all factors that
start, analysis, and final upper temperature hold time.
influence baseline stability, such as column bleed, septum
10.1.1 After chromatographic conditions have been set to
bleed, detector temperature control, constancy of carrier gas
meet performance requirements, program the column tempera-
flow, leaks, instrument drift, and so forth. Periodic baseline
ture upward to the maximum temperature to be used and hold
blank analyses should be made, following the analysis se-
that temperature for the selected time. Following the analysis
quence protocol, to give an indication of baseline stability.
sequence protocol, cool the column to the initial starting
NOTE 6—If automatic baseline correction (see Note 4) is provided by
temperature.
the gas chromatograph, further correction of area slices may not be
10.1.2 During the cool down and equilibration time, ready
required. However, if an electronic offset is added to the signal after
the integrator/computer system. If a retention time or detector
baseline compensation, additional area slice correction may be required in
response calibration is being performed, use the peak detection
the form of offset subtraction. Consult the specific instrumentation
mode. For samples and baseline compensation determinations, instructions to determine if an offset is applied to the signal. If the
D2887 − 23
algorithm used is unclear, the slice area data can be examined to determine
determination will be likely if column overloading occurs. The
if further correction is necessary. Determine if any offset has been added
column liquid phase loading has a direct bearing on acceptable
to the compensated signal by examining the corrected area slices of those
sample size. Reanalyze the calibration mixture using a smaller
time slices that precede the elution of any chromatographic unretained
sample size or a more dilute solution to avoid peak distortion.
substance. If these corrected area slices (representing the true baseline)
deviate from zero, subtract the average of these corrected area slices from 10.3.2 Prepare a calibration table based upon the results of
each corrected area slice in the analysis.
the analysis of the calibration mixture by recording the time of
each peak maximum and the boiling point temperature in
10.3 Retention Time Versus Boiling Point Calibration—In
degrees Celsius (or Fahrenheit) for every component in the
order to analyze samples, a retention time versus boiling point
mixture. n-Paraffin boiling point temperatures are listed in
calibration must be performed. Inject an appropriate aliquot
Table 2.
(0.2 μL to 2.0 μL) of the calibration mixture (see 7.8) into the
10.3.3 Plot the retention time of each peak versus the
chromatograph, using the analysis sequence protocol. Obtain a
normal (peak detection) data record in order to determine the corresponding normal boiling point temperature of that com-
ponent in degrees Celsius (or Fahrenheit) as shown in Fig. 2.
peak retention times and the peak areas for each component.
Collect a time slice area record if a boiling range distribution 10.3.4 Ideally, the retention time versus boiling point tem-
report is desired. perature calibration plot would be linear, but it is impractical to
10.3.1 Inspect the chromatogram of the calibration mixture operate the chromatograph such that curvature is eliminated
for evidence of skewed (non-Gaussian shaped) peaks. Skew- completely. The greatest potential for deviation from linearity
ness is often an indication of overloading the sample capacity will be associated with the lower boiling point paraffins. They
of the column that will result in displacement of the peak apex will elute from the column relatively fast and have the largest
relative to non-overloaded peaks. Distortion in retention time difference in boiling point temperature. In general, the lower
measurement and hence errors in boiling point temperature the sample IBP, the lower will be the starting temperature of
FIG. 2 Typical Calibration Curve
D2887 − 23
the analysis. Although extrapolation of the curve at the upper 12. Calculations
end is more accurate, calibration points must bracket the
12.1 Acquisition Rate Requirements:
boiling range of the sample at both the low and high ends.
12.1.1 The number of slices required at the beginning of
10.4 Reference Gas Oil Analysis—The reference gas oil data acquisition depends on chromatographic variables such as
the column flow, column film thickness, and initial column
sample is used to verify both the chromatographic and calcu-
lation processes involved in this test method. Perform an temperature as well as column length. In addition the detector
signal level has to be as low as possible at the initial
analysis of the gas oil following the analysis sequence proto-
col. Collect the area slice data and provide a boiling point temperature of the analysis. The detector signal level for both
the sample signal and the blank at the beginning of the run has
distribution report as in Sections 12 and 13.
to be similar for proper zeroing of the signals.
10.4.1 The results of this reference analysis must be within
12.1.2 The sampling frequency has to be adjusted so that at
the upper and lower limit values inclusively given in Table 3 or
least a significant number of slices are acquired prior to the
Table 4. If it does not meet the criteria in Table 3 or Table 4,
start of elution of sample or solvent. For example, if the time
check that all hardware is operating properly and all instrument
settings are as recommended by the manufacturer. Rerun the for start of sample elution is 0.06 min (3.6 s), a sampling rate
of 5 Hz would acquire 18 slices. However a rate of 1 Hz would
retention boiling point calibration as described in 10.3.
only acquire 3.6 slices which would not be sufficient for
10.4.2 Perform this reference gas oil confirmation test at
zeroing the signals. Rather than specifying number of slices, it
least once per day or as often as required to establish
is important to select an initial time segment that is, one or two
confidence in consistent compliance with 10.4.1.
seconds. Ensure that the smallest number of slices is 5 or
greater.
11. Procedure
12.1.3 Verify that the slice width used to acquire the sample
11.1 Sample Preparation:
chromatogram is the same used to acquire the blank run
11.1.1 The amount of sample injected must not overload the
chromatogram.
column stationary phase nor exceed the detector linear range. A
12.2 Chromatograms Offset for Sample and Blank—
narrow boiling range sample will require a smaller amount
Perform a slice offset for the sample chromatogram and blank
injected than a wider boiling range sample.
chromatogram. This operation is necessary so that the signal is
11.1.1.1 To determine the detector linear range, refer to
corrected from its displacement from the origin. This is
Practice E594 for flame ionization detectors or Practice E516
achieved by determining an average slice offset from the slices
for thermal conductivity detectors.
accumulated in the first segment (that is, first s) and performing
11.1.1.2 The column stationary phase capacity can be esti-
a standard deviation calculation for the first N slices accumu-
mated from the chromatogram of the calibration mixture (see
lated. It is carried out for both sample signal and baseline
9.3.2). Different volumes of the calibration standard can be
signal.
injected to find the maximum amount of a component that the
12.2.1 Sample Offset:
stationary phase can tolerate without overloading (see 10.3.1).
12.2.1.1 Calculate the average slice offset of sample chro-
Note the peak height for this amount of sample. The maximum
matogram using the first second of acquired slices. Insure that
sample signal intensity should not exceed this peak height.
no sample has eluted during this time and that the number of
11.1.2 Samples that are of low enough viscosity to be
slices acquired is at least 5. Throw out any of the first N slices
sampled with a syringe at ambient temperature may be injected
selected that are not within one standard deviation of the
neat. This type of sample may also be diluted with CS to
average and recompute the average. This eliminates any area
control the amount of sample injected to comply with 11.1.1.
that is due to possible baseline upset from injection.
11.1.3 Samples that are too viscous or waxy to sample with
12.2.1.2 Subtract the average slice offset from all the slices
a syringe may be diluted with CS .
of the sample chromatogram. Set negative slices to zero. This
11.1.4 Typical sample injection volumes are listed below.
will zero the chromatogram.
Packed Columns:
12.2.2 Blank Offset:
Stationary Phase Loading, % Neat Sample Volume, μL
10 1.0
NOTE 7—If you are using electronic baseline compensation proceed to
5 0.5
12.4. It is strongly recommende
...

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.
´1
Designation: D2887 − 22 D2887 − 23
Standard Test Method for
Boiling Range Distribution of Petroleum Fractions by Gas
Chromatography
This standard is issued under the fixed designation D2887; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.
ε NOTE—Editorially removed joint designation and corrected 13.1 in February 2023.
1. Scope*
1.1 This test method covers the determination of the boiling range distribution of petroleum products. The test method is
applicable to petroleum products and fractions having a final boiling point of 538 °C (1000 °F) or lower at atmospheric pressure
as measured by this test method. This test method is limited to samples having a boiling range greater than 55.5 °C (100 °F), and
having a vapor pressure sufficiently low to permit sampling at ambient temperature.
NOTE 1—Since a boiling range is the difference between two temperatures, only the constant of 1.8 °F ⁄°C is used in the conversion of the temperature
range from one system of units to another.
1.1.1 Procedure A (Sections 6 – 14)—Allows a larger selection of columns and analysis conditions such as packed and capillary
columns as well as a Thermal Conductivity Detector in addition to the Flame Ionization Detector. Analysis times range from
14 min to 60 min.
1.1.2 Procedure B (Sections 15 – 23)—Is restricted to only 3 capillary columns and requires no sample dilution. In addition,
Procedure B is used not only for the sample types described in Procedure A but also for the analysis of samples containing biodiesel
mixtures B5, B10, and B20. The analysis time, when using Procedure B (Accelerated D2887), is reduced to about 8 min.
1.2 This test method is not to be used for the analysis of gasoline samples or gasoline components. These types of samples must
be analyzed by Test Method D7096.
1.3 The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for
information only and are not considered 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.
This test method is under the jurisdiction of Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcommittee
D02.04.0H on Chromatographic Distribution Methods.
Current edition approved Sept. 1, 2022July 1, 2023. Published September 2022December 2023. Originally approved in 1973. Last previous edition approved in 20192022
ɛ2ɛ1
as D2887 – 19aD2887 – 22 . DOI: 10.1520/D2887-22E01.10.1520/D2887-23.
*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
D2887 − 23
2. Referenced Documents
2.1 ASTM Standards:
D86 Test Method for Distillation of Petroleum Products and Liquid Fuels at Atmospheric Pressure
D1160 Test Method for Distillation of Petroleum Products at Reduced Pressure
D2892 Test Method for Distillation of Crude Petroleum (15-Theoretical Plate Column)
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4175 Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants
D4626 Practice for Calculation of Gas Chromatographic Response Factors
D6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measure-
ment System Performance
D6300 Practice for Determination of Precision and Bias Data for Use in Test Methods for Petroleum Products, Liquid Fuels, and
Lubricants
D6708 Practice for Statistical Assessment and Improvement of Expected Agreement Between Two Test Methods that Purport
to Measure the Same Property of a Material
D7096 Test Method for Determination of the Boiling Range Distribution of Gasoline by Wide-Bore Capillary Gas
Chromatography
D7169 Test Method for Boiling Point Distribution of Samples with Residues Such as Crude Oils and Atmospheric and Vacuum
Residues by High Temperature Gas Chromatography
E29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
E260 Practice for Packed Column Gas Chromatography
E355 Practice for Gas Chromatography Terms and Relationships
E516 Practice for Testing Thermal Conductivity Detectors Used in Gas Chromatography
E594 Practice for Testing Flame Ionization Detectors Used in Gas or Supercritical Fluid Chromatography
3. Terminology
3.1 Definitions—This test method makes reference to many common gas chromatographic procedures, terms, and relationships.
Detailed definitions of these can be found in Practices E260, E355, and E594.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 area slice, n—the area, resulting from the integration of the chromatographic detector signal, within a specified retention
time interval. In area slice mode (see 6.3.2), peak detection parameters are bypassed and the detector signal integral is recorded
as area slices of consecutive, fixed duration time intervals.
3.2.2 corrected area slice, n—an area slice corrected for baseline offset, by subtraction of the exactly corresponding area slice in
a previously recorded blank (non-sample) analysis.
3.2.3 cumulative corrected area, n—the accumulated sum of corrected area slices from the beginning of the analysis through a
given retention time, ignoring any non-sample area (for example, solvent).
3.2.4 final boiling point (FBP), n—the temperature (corresponding to the retention time) at which a cumulative corrected area
count equal to 99.5 % of the total sample area under the chromatogram is obtained.
3.2.5 initial boiling point (IBP), n—the temperature (corresponding to the retention time) at which a cumulative corrected area
count equal to 0.5 % of the total sample area under the chromatogram is obtained.
3.2.6 slice rate, n—the time interval used to integrate the continuous (analog) chromatographic detector response during an
analysis. The slice rate is expressed in hertz (for example, integrations or slices per second).
3.2.7 slice time, n—the time associated with the end of each contiguous area slice. The slice time is equal to the slice number
divided by the slice rate.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
D2887 − 23
3.2.8 total sample area, n—the cumulative corrected area, from the initial area point to the final area point, where the
chromatographic signal is considered to have returned to baseline after complete sample elution.
3.3 Abbreviations:
3.3.1 A common abbreviation of hydrocarbon compounds is to designate the number of carbon atoms in the compound. A prefix
is used to indicate the carbon chain form, while a subscripted suffix denotes the number of carbon atoms (for example, normal
decane = n-C ; isotetradecane = i-C ).
10 14
4. Summary of Test Method
4.1 The boiling range distribution determination by distillation is simulated by the use of gas chromatography. A nonpolar packed
or open tubular (capillary) gas chromatographic column is used to elute the hydrocarbon components of the sample in order of
increasing boiling point. The column temperature is raised at a reproducible linear rate and the area under the chromatogram is
recorded throughout the analysis. Boiling points are assigned to the time axis from a calibration curve obtained under the same
chromatographic conditions by analyzing a known mixture of hydrocarbons covering the boiling range expected in the sample.
From these data, the boiling range distribution can be obtained.
4.2 Procedure A and Procedure B yield essentially the same results. See Sections 14 and 23, and the accompanying research
reports.
5. Significance and Use
5.1 The boiling range distribution of petroleum fractions provides an insight into the composition of feedstocks and products
related to petroleum refining processes. The gas chromatographic simulation of this determination can be used to replace
conventional distillation methods for control of refining operations. This test method can be used for product specification testing
with the mutual agreement of interested parties.
5.2 Boiling range distributions obtained by this test method are essentially equivalent to those obtained by true boiling point (TBP)
distillation (see Test Method D2892). They are not equivalent to results from low efficiency distillations such as those obtained
with Test Method D86 or D1160.
5.3 Procedure B was tested with biodiesel mixtures and reports the Boiling Point Distribution of FAME esters of vegetable and
animal origin mixed with ultra low sulfur diesel.
Procedure A
6. Apparatus
6.1 Chromatograph—The gas chromatograph used must have the following performance characteristics:
6.1.1 Detector—Either a flame ionization or a thermal conductivity detector may be used. The detector must have sufficient
sensitivity to detect 1.0 % dodecane with a peak height of at least 10 % of full scale on the recorder under conditions prescribed
in this test method and without loss of resolution as defined in 9.3.1. When operating at this sensitivity level, detector stability must
be such that a baseline drift of not more than 1 % of full scale per hour is obtained. The detector must be capable of operating
continuously at a temperature equivalent to the maximum column temperature employed. Connection of the column to the detector
must be such that no temperature below the column temperature exists.
NOTE 2—It is not desirable to operate a thermal conductivity detector at a temperature higher than the maximum column temperature employed. Operation
at higher temperature generally contributes to higher noise levels and greater drift and can shorten the useful life of the detector.
6.1.2 Column Temperature Programmer—The chromatograph must be capable of linear programmed temperature operation over
a range sufficient to establish a retention time of at least 1 min for the IBP and to elute compounds up to a boiling temperature
of 538 °C (1000 °F) before reaching the upper end of the temperature program. The programming rate must be sufficiently
reproducible to obtain retention time repeatability of 0.1 min (6 s) for each component in the calibration mixture described in 7.8.
D2887 − 23
6.1.3 Cryogenic Column Cooling—Column starting temperatures below ambient will be required if samples with IBPs of less than
93 °C (200 °F) are to be analyzed. This is typically provided by adding a source of either liquid carbon dioxide or liquid nitrogen,
controlled through the oven temperature circuitry. Excessively low initial column temperature must be avoided to ensure that the
stationary phase remains liquid. The initial temperature of the column should be only low enough to obtain a calibration curve
meeting the specifications of the method.
6.1.4 Sample Inlet System—The sample inlet system must be capable of operating continuously at a temperature equivalent to the
maximum column temperature employed, or provide for on-column injection with some means of programming the entire column,
including the point of sample introduction, up to the maximum temperature required. Connection of the column to the sample inlet
system must be such that no temperature below the column temperature exists.
6.1.5 Flow Controllers—The gas chromatograph must be equipped with mass flow controllers capable of maintaining carrier gas
flow constant to 61 % over the full operating temperature range of the column. The inlet pressure of the carrier gas supplied to
the gas chromatograph must be sufficiently high to compensate for the increase in column backpressure as the column temperature
is raised. An inlet pressure of 550 kPa (80 psig) has been found satisfactory with the packed columns described in Table 1. For
open tubular columns, inlet pressures from 10 kPa to 70 kPa (1.5 psig to 10 psig) have been found to be suitable.
6.1.6 Microsyringe—A microsyringe is needed for sample introduction.
NOTE 3—Automatic sampling devices or other sampling means, such as indium encapsulation, can be used provided: the system can be operated at a
temperature sufficiently high to completely vaporize hydrocarbons with atmospheric boiling points of 538 °C (1000 °F), and the sampling system is
connected to the chromatographic column avoiding any cold temperature zones.
TABLE 1 Typical Operating Conditions for Procedure A
Packed Columns 1 2 3 4 Open Tubular Columns 5 6 7
Column length, m (ft) 1.2 (4) 1.5 (5) 0.5 (1.5) 0.6 (2) Column length (m) 7.5 5 10
Column length, m (ft) 1.2 (4) 1.5 (5) 0.5 (1.5) 0.6 (2) Column length (m) 5 10
Column outside diameter, mm 6.4 (1/4) 3.2 (1/8) 3.2 (1/8) 6.4 (1/8) Column inner diameter (mm) 0.53 0.53 0.53
(in.)
Column outside diameter, mm 6.4 (1/4) 3.2 (1/8) 3.2 (1/8) 6.4 (1/8) Column inner diameter (mm) 0.53 0.53
(in.)
Liquid phase OV-1 SE-30 UC-W98 SE-30 Stationary phase DB-1 HP-1 HP-1
Liquid phase OV-1 SE-30 UC-W98 SE-30 Stationary phase HP-1 HP-1
Percent liquid phase 3 5 10 10 Stationary phase thickness 1.5 0.88 2.65
(m)
Percent liquid phase 3 5 10 10 Stationary phase thickness 0.88 2.65
(μm)
A B C C D
Support material S G P P Carrier gas nitrogen helium helium
A B C C
Support material S G P P Carrier gas helium helium
Support mesh size 60/80 60/80 80/100 60/80 Carrier gas flow rate, mL/min 30 12 12
Support mesh size 60/80 60/80 80/100 60/80 Carrier gas flow rate, mL/min 12 12
Initial column temperature, °C –20 –40 –30 –50 Initial column temperature, °C 40 35 35
Initial column temperature, °C –20 –40 –30 –50 Initial column temperature, °C 35 35
Final column temperature, °C 360 350 360 390 Final column temperature, °C 340 350 350
Final column temperature, °C 360 350 360 390 Final column temperature, °C 350 350
Programming rate, °C/min 10 6.5 10 7.5 Programming rate, °C/min 10 10 20
Programming rate, °C/min 10 6.5 10 7.5 Programming rate, °C/min 10 20
Carrier gas helium helium N helium Detector FID FID FID
Carrier gas helium helium N helium Detector FID FID
Carrier gas flow, mL/min 40 30 25 60 Detector temperature, °C 350 380 370
Carrier gas flow, mL/min 40 30 25 60 Detector temperature, °C 380 370
Detector TC FID FID TC Injector temperature, °C 340 cool on-column cool on-column
Detector TC FID FID TC Injector temperature, °C cool on-column cool on-column
Detector temperature, °C 360 370 360 390 Sample size, μL 0.5 1 0.1–0.2
Detector temperature, °C 360 370 360 390 Sample size, μL 1 0.1–0.2
Injection port temperature, °C 360 370 350 390 Sample concentration mass % 25 2 neat
Injection port temperature, °C 360 370 350 390 Sample concentration mass % 2 neat
Sample size, μ 4 0.3 1 5
A
Diatoport S; silane treated.
B
Chromosorb G (AW-DMS).
C
Chromosorb P, acid washed.
D
There is no precision study using nitrogen as carrier.
D2887 − 23
6.2 Column—Any column and conditions may be used that provide separation of typical petroleum hydrocarbons in order of
increasing boiling point and meet the column performance requirements of 9.3.1 and 9.3.3. Successfully used columns and
conditions are given in Table 1.
6.3 Data Acquisition System:
6.3.1 Recorder—A 0 mV to 1 mV range recording potentiometer or equivalent, with a full-scale response time of 2 s or less may
be used.
6.3.2 Integrator—Means must be provided for determining the accumulated area under the chromatogram. This can be done by
means of an electronic integrator or computer-based chromatography data system. The integrator/computer system must have
normal chromatographic software for measuring the retention time and areas of eluting peaks (peak detection mode). In addition,
the system must be capable of converting the continuously integrated detector signal into area slices of fixed duration. These
contiguous area slices, collected for the entire analysis, are stored for later processing. The electronic range of the
integrator/computer (for example, 1 V, 10 V) must be within the linear range of the detector/electrometer system used. The system
must be capable of subtracting the area slice of a blank run from the corresponding area slice of a sample run.
NOTE 4—Some gas chromatographs have an algorithm built into their operating software that allows a mathematical model of the baseline profile to be
stored in memory. This profile is automatically subtracted from the detector signal on subsequent sample analyses to compensate for any baseline offset.
Some integration systems also store and automatically subtract a blank analysis from subsequent analytical determinations.
7. Reagents and Materials
7.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society where such
specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity
to permit its use without lessening the accuracy of the determination.
7.2 Liquid Phase for Columns—Methyl silicone gums and liquids provide the proper chromatographic hydrocarbon elution
characteristics for this test method.
7.3 Solid Support for Packed Columns—Chromatographic grade diatomateous earth solid support material within a particle size
range from 60 to 100 sieve mesh size is recommended.
7.4 Carrier Gas—Helium or nitrogen of high purity. purity (99.999 % pure). (Warning—Helium is a compressed gasand nitrogen
are compressed gases under high pressure.) Additional purification is recommended by the use of molecular sieves or other suitable
agents to remove water, oxygen, and hydrocarbons. The use of helium and nitrogen as carrier gas have valid precision statements.
The precision for using nitrogen as carrier gas is described in Annex A2. Available pressure must be sufficient to ensure a constant
carrier gas flow rate (see 6.1.5). Appendix X5 lists conditions for using hydrogen and nitrogen as carriers as carrier gas for
Procedure A. Note X5.1 also states that results with these alternative carriers are not considered to be valid D2887 Procedure A
results until a valid precision (r and R) statement is obtaind from an ILS using Procedure A is carried out.A.
7.5 Hydrogen—Hydrogen of high purity (for example, hydrocarbon free) (99.999 % pure) is used as fuel for the flame ionization
detector (FID). (Warning—Hydrogen is an extremely flammable gas under high pressure.)
7.6 Air—High purity (for example, hydrocarbon free) compressed air is used as the oxidant for the flame ionization detector (FID).
(Warning—Compressed air is a gas under high pressure and supports combustion.)
7.7 Column Resolution Test Mixture—For packed columns, a nominal mixture of 1 % by mass each of n-C and n-C paraffin
16 18
in a suitable solvent, such as n-octane, for use in testing the column resolution. (Warning—n-octane is flammable and harmful
ACS Reagent Chemicals, Specifications and Procedures for Reagents and Standard-Grade Reference Materials, American Chemical Society, Washington, DC. For
suggestions on the testing of reagents not listed by the American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and
the United States Pharmacopeia and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
D2887 − 23
if inhaled.) The calibration mixture specified in 7.8.2 may be used as a suitable alternative, provided the concentrations of the n-C
and n-C components are nominally 1.0 % by mass each. For open tubular columns, use the mixture specified in 7.8.3.
7.8 Calibration Mixture—An accurately weighed mixture of approximately equal mass quantities of n-hydrocarbons dissolved in
carbon disulfide (CS ). (Warning—Carbon disulfide is extremely volatile, flammable, and toxic.) The mixture shall cover the
boiling range from n-C to n-C , but does not need to include every carbon number (see Note 5).
5 44
7.8.1 At least one compound in the mixture must have a boiling point lower than the IBP of the sample and at least one compound
in the mixture must have a boiling point higher than the FBP of the sample. Boiling points of n-paraffins are listed in Table 2.
7.8.1.1 If necessary, for the calibration mixture to have a compound with a boiling point below the IBP of the sample, propane
or butane can be added to the calibration mixture, non-quantitatively, by bubbling the gaseous compound into the calibration
mixture in a septum sealed vial using a gas syringe.
NOTE 5—Calibration mixtures containing normal paraffins with the carbon numbers 5, 6, 7, 8, 9, 10, 11, 12, 14, 15, 16, 17, 18, 20, 24, 28, 32, 36, 40,
and 44 have been found to provide a sufficient number of points to generate a reliable calibration curve.
7.8.2 Packed Columns—The final concentration should be approximately ten parts of the n-paraffin mixture to one hundred parts
of CS .
7.8.3 Open Tubular Columns—The final concentration should be approximately one part of the n-paraffin mixture to one hundred
parts of CS .
A, B, C
TABLE 2 Boiling Points of Normal Paraffins
Carbon Boiling Boiling Carbon Boiling Boiling
Number Point, °C Point, °F Number Point, °C Point, °F
1 –162 –259 23 380 716
2 –89 –127 24 391 736
3 –42 –44 25 402 755
4 0 31 26 412 774
5 36 97 27 422 791
6 69 156 28 431 808
7 98 209 29 440 825
8 126 258 30 449 840
9 151 303 31 458 856
10 174 345 32 466 870
11 196 385 33 474 885
12 216 421 34 481 898
13 235 456 35 489 912
14 254 488 36 496 925
15 271 519 37 503 937
16 287 548 38 509 948
17 302 576 39 516 961
18 316 601 40 522 972
19 330 626 41 528 982
20 344 651 42 534 993
21 356 674 43 540 1004
22 369 695 44 545 1013
A
API Project 44, October 31, 1972 is believed to have provided the original normal
paraffin boiling point data that are listed in Table 2. However, over the years some
of the data contained in both API Project 44 (Thermodynamics Research Center
Hydrocarbon Project) and Test Method D2887 have changed, and they are no
longer equivalent. Table 2 represents the current normal paraffin boiling point
values accepted by Subcommittee D02.04 and found in all test methods under the
jurisdiction of Section D02.04.0H.
B
Test Method D2887 has traditionally used n-paraffin boiling points rounded to the
nearest whole degree for calibration. The boiling points listed in Table 2 are correct
to the nearest whole number in both degrees Celsius and degrees Fahrenheit.
However, if a conversion is made from one unit to the other and then rounded to
a whole number, the result will not agree with the table value for a few carbon
numbers. For example, the boiling point of n-heptane is 98.425 °C, which is
correctly rounded to 98 °C in the table. However, converting 98.425 °C gives
209.165 °F, which rounds to 209 °F, while converting 98 °C gives 208.4 °F, which
rounds to 208 °F. Carbon numbers 2, 4, 7, 8, 9, 13, 14, 15, 16, 25, 27, and 32 are
affected by rounding.
C
Table X6.1 lists the current boiling points of n-paraffins approved by API.
D2887 − 23
7.9 Reference Gas Oil (Tables 3 and 4)—A reference material that has been analyzed by laboratories participating in the test
method cooperative study. Accepted Reference Values (ARV) for the boiling range distribution of these reference oils are given
in Tables 3 and 4. Addition of new reference material to this standard requires the ARV of the new reference material to be
determined in accordance with a similar cooperative study using a minimum participation of 16 laboratories as described in
Practice D6299 (6.2.2.1) for determination of check standard ARV using interlaboratory testing. Results for the new reference
material provided by each laboratory shall be validated by an accompanying qualifying result using a current reference oil in this
standard.
8. Sampling
8.1 Samples to be analyzed by this test method must be obtained using the procedures outlined in Practice D4057.
8.2 The test specimen to be analyzed must be homogeneous and free of dust or undissolved material.
9. Preparation of Apparatus
9.1 Chromatograph—Place in service in accordance with the manufacturer’s instructions. Typical operating conditions are shown
in Table 1.
9.1.1 When a FID is used, regularly remove the deposits formed in the detector from combustion of the silicone liquid phase
decomposition products. These deposits will change the response characteristics of the detector.
A, B
TABLE 3 Test Method D2887 Reference Gas Oil No. 1
ARV RGO No. 1 Batch 1 ARV RGO No. 1 Batch 2 ARV RGO No. 1 Batch 3
Mid- Allowed Mid- Allowed Mid- Allowed
% OFF Lower Upper point Devia- Lower Upper point Devia- Lower Upper point Devia- % OFF
Limit Limit Value tion Limit Limit Value tion Limit Limit Value tion
(°F) (°F) (°F) (°F) (°F) (°F) (°F) (°F) (°F) (°F) (°F) (°F)
IBP 224.4 251.6 238.0 13.6 225.8 253.2 239.5 13.7 224.2 251.4 237.8 13.6 IBP
5 282.4 295.6 289.0 6.6 297.4 311.0 304.2 6.8 296.8 310.4 303.6 6.8 5
10 328.7 343.3 336.0 7.3 341.2 356.0 348.6 7.4 338.8 353.6 346.2 7.4 10
20 420.3 437.7 429.0 8.7 426.0 443.4 434.7 8.7 431.4 449.0 440.2 8.8 20
30 487.6 504.4 496.0 8.4 490.2 507.0 498.6 8.4 502.4 519.5 510.9 8.6 30
40 540.3 555.7 548.0 7.7 544.4 559.8 552.1 7.7 554.8 570.2 562.5 7.7 40
50 586.3 601.7 594.0 7.7 586.1 601.5 593.8 7.7 593.2 608.6 600.9 7.7 50
60 621.3 636.7 629.0 7.7 621.3 636.7 629.0 7.7 628.5 643.9 636.2 7.7 60
70 661.3 676.7 669.0 7.7 661.0 676.4 668.7 7.7 667.3 682.7 675.0 7.7 70
80 701.3 716.7 709.0 7.7 704.5 719.9 712.2 7.7 713.0 728.4 720.7 7.7 80
90 751.3 766.7 759.0 7.7 756.6 772.0 764.3 7.7 764.9 780.3 772.6 7.7 90
95 788.0 806.0 797.0 9.0 794.0 812.0 803.0 9.0 799.5 817.5 808.5 9.0 95
FBP 865.8 908.2 887.0 21.2 866.1 908.5 887.3 21.2 853.5 895.9 874.7 21.2 FBP
ARV RGO No. 1 Batch 1 ARV RGO No. 1 Batch 2 ARV RGO No. 1 Batch 3
Mid- Allowed Mid- Allowed Mid- Allowed
% OFF Lower Upper point Devia- Lower Upper point Devia- Lower Upper point Devia- % OFF
Limit Limit Value tion Limit Limit Value tion Limit Limit Value tion
(°C) (°C) (°C) (°C) (°C) (°C) (°C) (°C) (°C) (°C) (°C) (°C)
IBP 106.9 122.0 114.4 7.6 107.7 122.9 115.3 7.6 106.8 121.9 114.3 7.5 IBP
5 139.1 146.4 142.8 3.6 147.5 155.0 151.2 3.8 147.1 154.6 150.9 3.8 5
10 164.9 172.9 168.9 4.0 171.8 180.0 175.9 4.1 170.4 178.7 174.6 4.1 10
20 215.7 225.4 220.6 4.8 218.9 228.6 223.7 4.9 221.9 231.7 226.8 4.9 20
30 253.1 262.4 257.8 4.7 254.6 263.9 259.2 4.7 261.3 270.8 266.1 4.8 30
40 282.4 290.9 286.7 4.3 284.7 293.2 288.9 4.3 290.4 299.0 294.7 4.3 40
50 307.9 316.5 312.2 4.3 307.8 316.4 312.1 4.3 311.8 320.3 316.0 4.3 50
60 327.4 335.9 331.7 4.3 327.4 335.9 331.7 4.3 331.4 340.0 335.7 4.3 60
70 349.6 358.2 353.9 4.3 349.4 358.0 353.7 4.3 353.0 361.5 357.2 4.3 70
80 371.8 380.4 376.1 4.3 373.6 382.2 377.9 4.3 378.3 386.9 382.6 4.3 80
90 399.6 408.2 403.9 4.3 402.6 411.1 406.8 4.3 407.2 415.7 411.4 4.3 90
95 420.0 430.0 425.0 5.0 423.3 433.3 428.3 5.0 426.4 436.4 431.4 5.0 95
FBP 463.2 486.8 475.0 11.8 463.4 486.9 475.2 11.8 456.4 480.0 468.2 11.8 FBP
A
Consensus results for Batch 2 obtained from 30 laboratories in 1995 (supporting data have been filed at ASTM International Headquarters and may be obtained by
requesting Research Report RR:D02-1407. Contact ASTM Customer Service at [e-mail].).
B
Supporting data for Batch 3 have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:D02-1913. Contact ASTM
Customer Service at [e-mail].
D2887 − 23
A
TABLE 4 Test Method D2887 Reference Gas Oil No. 2
ARV RGO No. 2 ARV RGO No. 2
Allowed Allowed
% OFF % OFF
Lower Limit Upper Limit Midpoint Value Deviation Lower Limit Upper Limit Midpoint Value Deviation
(°F) (°F) (°F) (°F) (°C) (°C) (°C) (°C)
IBP 209.6 234.7 222.2 12.6 98.7 112.6 105.7 7.0 IBP
5 335.1 349.8 342.5 7.4 168.4 176.6 172.5 4.1 5
10 376.3 392.2 384.2 8.0 191.3 200.1 195.7 4.4 10
20 442.7 460.7 451.7 9.0 228.2 238.2 233.2 5.0 20
30 503.4 520.6 512.0 8.6 261.9 271.4 266.7 4.8 30
40 559.9 575.3 567.6 7.7 293.3 301.9 297.6 4.3 40
50 601.6 617.0 609.3 7.7 316.4 325.0 320.7 4.3 50
60 638.8 654.2 646.5 7.7 337.1 345.6 341.4 4.3 60
70 669.4 684.8 677.1 7.7 354.1 362.7 358.4 4.3 70
80 704.3 719.7 712.0 7.7 373.5 382.0 377.8 4.3 80
90 755.3 770.7 763.0 7.7 401.9 410.4 406.1 4.3 90
95 799.0 817.0 808.0 9.0 426.1 436.1 431.1 5.0 95
FBP 905.3 947.7 926.5 21.2 485.2 508.7 496.9 11.8 FBP
A
Consensus results for Reference Gas Oil No. 2 obtained from 32 laboratories in 2009.
9.1.2 If the sample inlet system is heated above 300 °C (572 °F), a blank analysis must be made after a new septum is installed
to ensure that no extraneous detector response is produced by septum bleed. At the sensitivity levels commonly employed in this
test method, conditioning of the septum at the operating temperature of the sample inlet system for several hours will minimize
this problem. A recommended practice is to change the septum at the end of a series of analyses rather than at the beginning of
the series.
9.2 Column Preparation:
9.2.1 Packed Columns—Any satisfactory method that will produce a column meeting the requirements of 9.3.1 and 9.3.3 can be
used. In general, use liquid phase loadings of 3 % to 10 %. Condition the column at the maximum operating temperature to reduce
baseline shifts due to bleeding of the column substrate. The column can be conditioned very rapidly and effectively using the
following procedure:
9.2.1.1 Connect the column to the inlet but leave the detector end free.
9.2.1.2 Purge the column thoroughly at ambient temperature with carrier gas.
9.2.1.3 Turn off the carrier gas and allow the column to depressurize completely.
9.2.1.4 Seal off the open end (detector) of the column with an appropriate fitting.
9.2.1.5 Raise the column temperature to the maximum operating temperature.
9.2.1.6 Hold the column at this temperature for at least 1 h with no flow through the column.
9.2.1.7 Cool the column to ambient temperature.
9.2.1.8 Remove the cap from the detector end of the column and turn the carrier gas back on.
9.2.1.9 Program the column temperature up to the maximum several times with normal carrier gas flow. Connect the free end of
the column to the detector.
9.2.1.10 An alternative method of column conditioning that has been found effective for columns with an initial loading of 10 %
liquid phase consists of purging the column with carrier gas at the normal flow rate while holding the column at the maximum
operating temperature for 12 h to 16 h, while detached from the detector.
9.2.2 Open Tubular Columns—Open tubular columns with cross-linked and bonded stationary phases are available from many
manufacturers and are usually pre-conditioned. These columns have much lower column bleed than packed columns. Column
conditioning is less critical with these columns but some conditioning may be necessary. The column can be conditioned very
rapidly and effectively using the following procedure.
D2887 − 23
9.2.2.1 Once the open tubular column has been properly installed into the gas chromatograph and tested to be leak free, set the
column and detector gas flows. Before heating the column, allow the system to purge with carrier gas at ambient temperature for
at least 30 min.
9.2.2.2 Increase the oven temperature about 5 °C to 10 °C per minute to the final operating temperature and hold for about 30 min.
9.2.2.3 Cycle the gas chromatograph several times through its temperature program until a stable baseline is obtained.
9.3 System Performance Specification:
9.3.1 Column Resolution—The column resolution, influenced by both the column physical parameters and operating conditions,
affects the overall determination of boiling range distribution. Resolution is therefore specified to maintain equivalence between
different systems (laboratories) employing this test method. Resolution is determined using Eq 1 and the C and C paraffins from
16 18
a column resolution test mixture analysis (see 7.7 and Section 10), and is illustrated in Fig. 1. Resolution (R) should be at least
three, using the identical conditions employed for sample analyses:
R 5 2~t 2 t !/@1.699~w 1w !# (1)
2 1 2 1
where:
R = resolution,
t = time(s) for the n-C peak maximum,
1 16
t = time(s) for the n-C peak maximum,
2 18
w = peak width(s), at half height, of the n-C peak, and
1 16
w = peak width(s), at half height, of the n-C peak.
2 18
9.3.2 Detector Response Calibration—This test method assumes that the detector response to petroleum hydrocarbons is
proportional to the mass of individual components. This must be verified when the system is put in service, and whenever any
changes are made to the system or operational parameters. Analyze the calibration mixture using the identical procedure to be used
for the analysis of samples (see Section 10). Calculate the relative response factor for each n-paraffin (relative to n-decane) in
accordance with Practice D4626 and Eq 2:
F 5 ~M /A !/~M /A ! (2)
n n n 10 10
where:
F = relative response factor,
n
M = mass of the n-paraffin in the mixture,
n
A = peak area of the n-paraffin in the mixture,
n
FIG. 1 Column Resolution Parameters
D2887 − 23
M = mass of the n-decane in the mixture, and
A = peak area of the n-decane in the mixture.
The relative response factor (F ) of each n-paraffin must not deviate from unity (1) by more than 610 %.
n
9.3.3 Column Elution Characteristics—The column material, stationary phase, or other parameters can affect the elution order of
non-paraffinic sample components, resulting in deviations from a TBP versus retention time relationship. If stationary phases other
than those referenced in 7.3 are used, the retention times of a few alkylbenzenes (for example, o-xylene, n-butyl-benzene,
1,3,5-triisopropylbenzene, n-decyl-benzene, and tetradecylbenzene) across the boiling range should be analyzed to make certain
that the column is separating in accordance with the boiling point order (see Appendix X1).
10. Calibration and Standardization
10.1 Analysis Sequence Protocol—Define and use a predetermined schedule of analysis events designed to achieve maximum
reproducibility for these determinations. The schedule will include cooling the column oven to the initial starting temperature,
equilibration time, sample injection and system start, analysis, and final upper temperature hold time.
10.1.1 After chromatographic conditions have been set to meet performance requirements, program the column temperature
upward to the maximum temperature to be used and hold that temperature for the selected time. Following the analysis sequence
protocol, cool the column to the initial starting temperature.
10.1.2 During the cool down and equilibration time, ready the integrator/computer system. If a retention time or detector response
calibration is being performed, use the peak detection mode. For samples and baseline compensation determinations, use the area
slice mode of integration. The recommended slice rate for this test method is given in 12.1.2. Other slice rates may be used if within
the limits of 0.02 % and 0.2 % of the retention time of the final calibration component (C ). Larger slice rates may be used, as
may be required for other reasons, if provision is made to accumulate (bunch) the slice data to within these limits prior to
determination of the boiling range distribution.
10.1.3 At the exact time set by the schedule, inject either the calibration mixture or sample into the chromatograph; or make no
injection (baseline blank). At the time of injection, start the chromatograph time cycle and the integrator/computer data acquisition.
Follow the analysis sequence protocol for all subsequent repetitive analyses or calibrations. Since complete resolution of sample
peaks is not expected, do not change the detector sensitivity setting during the analysis.
10.2 Baseline Compensation Analysis—A baseline compensation analysis, or baseline blank, is performed exactly like an analysis
except no injection is made. A blank analysis must be performed at least once per day. The blank analysis is necessary due to the
usual occurrence of chromatographic baseline instability and is subtracted from sample analyses to remove any non-sample slice
area from the chromatographic data. The blank analysis is typically performed prior to sample analyses, but may be useful if
determined between samples or at the end of a sample sequence to provide additional data regarding instrument operation or
residual sample carryover from previous sample analyses. Attention must be given to all factors that influence baseline stability,
such as column bleed, septum bleed, detector temperature control, constancy of carrier gas flow, leaks, instrument drift, and so
forth. Periodic baseline blank analyses should be made, following the analysis sequence protocol, to give an indication of baseline
stability.
NOTE 6—If automatic baseline correction (see Note 4) is provided by the gas chromatograph, further correction of area slices may not be required.
However, if an electronic offset is added to the signal after baseline compensation, additional area slice correction may be required in the form of offset
subtraction. Consult the specific instrumentation instructions to determine if an offset is applied to the signal. If the algorithm used is unclear, the slice
area data can be examined to determine if further correction is necessary. Determine if any offset has been added to the compensated signal by examining
the corrected area slices of those time slices that precede the elution of any chromatographic unretained substance. If these corrected area slices
(representing the true baseline) deviate from zero, subtract the average of these corrected area slices from each corrected area slice in the analysis.
10.3 Retention Time Versus Boiling Point Calibration—In order to analyze samples, a retention time versus boiling point
calibration must be performed. Inject an appropriate aliquot (0.2 μL to 2.0 μL) of the calibration mixture (see 7.8) into the
chromatograph, using the analysis sequence protocol. Obtain a normal (peak detection) data record in order to determine the peak
retention times and the peak areas for each component. Collect a time slice area record if a boiling range distribution report is
desired.
10.3.1 Inspect the chromatogram of the calibration mixture for evidence of skewed (non-Gaussian shaped) peaks. Skewness is
often an indication of overloading the sample capacity of the column that will result in displacement of the peak apex relative to
non-overloaded peaks. Distortion in retention time measurement and hence errors in boiling point temperature determination will
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be likely if column overloading occurs. The column liquid phase loading has a direct bearing on acceptable sample size. Reanalyze
the calibration mixture using a smaller sample size or a more dilute solution to avoid peak distortion.
10.3.2 Prepare a calibration table based upon the results of the analysis of the calibration mixture by recording the time of each
peak maximum and the boiling point temperature in degrees Celsius (or Fahrenheit) for every component in the mixture. n-Paraffin
boiling point temperatures are listed in Table 2.
10.3.3 Plot the retention time of each peak versus the corresponding normal boiling point temperature of that component in
degrees Celsius (or Fahrenheit) as shown in Fig. 2.
10.3.4 Ideally, the retention time versus boiling point temperature calibration plot would be linear, but it is impractical to operate
the chromatograph such that curvature is eliminated completely. The greatest potential for deviation from linearity will be
associated with the lower boiling point paraffins. They will elute from the column relatively fast and have the largest difference
in boiling point temperature. In general, the lower the sample IBP, the lower will be the starting temperature of the analysis.
Although extrapolation of the curve at the upper end is more accurate, calibration points must bracket the boiling range of the
sample at both the low and high ends.
10.4 Reference Gas Oil Analysis—The reference gas oil sample is used to verify both the chromatographic and calculation
processes involved in this test method. Perform an analysis of the gas oil following the analysis sequence protocol. Collect the area
slice data and provide a boiling point distribution report as in Sections 12 and 13.
FIG. 2 Typical Calibration Curve
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10.4.1 The results of this reference analysis must be within the upper and lower limit values inclusively given in Table 3 or Table
4. If it does not meet the criteria in Table 3 or Table 4, check that all hardware is operating properly and all instrument settings
are as recommended by the manufacturer. Rerun the retention boiling point calibration as described in 10.3.
10.4.2 Perform this reference gas oil confirmation test at least once per day or as often as required to establish confidence in
consistent compliance with 10.4.1.
11. Procedure
11.1 Sample Preparation:
11.1.1 The amount of sample injected must not overload the column stationary phase nor exceed the detector linear range. A
narrow boiling range sample will require a smaller amount injected than a wider boiling range sample.
11.1.1.1 To determine the detector linear range, refer to Practice E594 for flame ionization detectors or Practice E516 for thermal
conductivity detectors.
11.1.1.2 The column stationary phase capacity can be estimated from the chromatogram of the calibration mixture (see 9.3.2).
Different volumes of the calibration standard can be injected to find the maximum amount of a component that the stationary phase
can tolerate without overloading (see 10.3.1). Note the peak height for this amount of sample. The maximum sample signal
intensity should not exceed this peak height.
11.1.2 Samples that are of low enough viscosity to be sampled with a syringe at ambient temperature may be injected neat. This
type of sample may also be diluted with CS to control the amount of sample injected to comply with 11.1.1.
11.1.3 Samples that are too viscous or waxy to sample with a syringe may be diluted with CS .
11.1.4 Typical sample injection volumes are listed below.
Packed Columns:
Stationary Phase Loading, % Neat Sample Volume, μL
10 1.0
5 0.5
Open Tubular Columns:
Film Thickness, μ Neat Sample Volume, μL
0.8 to 1.5 0.1 to 0.2
1.8 to 3.0 0.1 to 0.5
3.0 to 5.0 0.2 to 1.0
11.2 Sample Analysis—Using the analysis sequence protocol, inject a sample aliquot into the gas chromatograph. Collect a
contiguous time slice area record of the entire analysis.
12. Calculations
12.1 Acquisition Rate Requirements:
12.1.1 The number of slices required at the beginning of data acquisition depends on chromatographic variables such as the
column flow, column film thickness, and initial column temperature as well as column length. In addition the detector signal level
has to be as low as possible at the initial temperature of the analysis. The detector signal level for both the sample signal and the
blank at the beginning o
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