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ASTM D3239-91(2011)

(Test Method)

Standard Test Method for Aromatic Types Analysis of Gas-Oil Aromatic Fractions by High Ionizing Voltage Mass Spectrometry

Standard Test Method for Aromatic Types Analysis of Gas-Oil Aromatic Fractions by High Ionizing Voltage Mass Spectrometry

SIGNIFICANCE AND USE
A knowledge of the hydrocarbon composition of process streams and petroleum products boiling within the range 205 to 540°C (400 to 1000°F) is useful in following the effect of changes in process variables, diagnosing the source of plant upsets, and in evaluating the effect of changes in composition on product performance properties. This method, when used together with Test Method D2786, provides a detailed analysis of the hydrocarbon composition of such materials.
SCOPE
1.1 This test method covers the determination by high ionizing voltage, low resolution mass spectrometry of 18 aromatic hydrocarbon types and 3 aromatic thiophenotypes in straight run aromatic petroleum fractions boiling within the range from 205 to 540°C (400 to 1000°F) (corrected to atmospheric pressure). Samples must be nonolefinic, must contain not more than 1 mass % of total sulfur, and must contain not more than 5 % nonaromatic hydrocarbons. Composition data are in volume percent.
Note 1—Although names are given to 15 of the compound types determined, the presence of other compound types of the same empirical formulae is not excluded. All other compound types in the sample, unidentified by name or empirical formula, are lumped into six groups in accordance with their respective homologous series.  
1.2 The values stated in acceptable SI units are to be regarded as the standard. The values given in parentheses are provided for information purposes only.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

General Information

Status
Historical
Publication Date
30-Sep-2011
ICS
75.080 - Petroleum products in general
Technical Committee
D02 - Petroleum Products, Liquid Fuels, and Lubricants
Drafting Committee
D02.04.0M - Mass Spectrometry
Current Stage
Ref Project

Relations

Replaces
ASTM D3239-91(2006) - Standard Test Method for Aromatic Types Analysis of Gas-Oil Aromatic Fractions by High Ionizing Voltage Mass Spectrometry
Effective Date
01-Oct-2011
Referred By
ASTM D2549-23 - Standard Test Method for Separation of Representative Aromatics and Nonaromatics Fractions of High-Boiling Oils by Elution Chromatography
Effective Date
01-Oct-2011

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ASTM D3239-91(2011) - Standard Test Method for Aromatic Types Analysis of Gas-Oil Aromatic Fractions by High Ionizing Voltage Mass SpectrometryASTM D3239-91(2011) - Standard Test Method for Aromatic Types Analysis of Gas-Oil Aromatic Fractions by High Ionizing Voltage Mass Spectrometry
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ASTM D3239-91(2011) - Standard Test Method for Aromatic Types Analysis of Gas-Oil Aromatic Fractions by High Ionizing Voltage Mass Spectrometry
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D3239 − 91(Reapproved 2011)
Standard Test Method for
Aromatic Types Analysis of Gas-Oil Aromatic Fractions by
High Ionizing Voltage Mass Spectrometry
This standard is issued under the fixed designation D3239; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope Gas-Oil Saturates Fractions by High Ionizing Voltage
2 Mass Spectrometry
1.1 This test method covers the determination by high
E137Practice for Evaluation of Mass Spectrometers for
ionizing voltage, low resolution mass spectrometry of 18
Quantitative Analysis from a Batch Inlet (Withdrawn
aromatic hydrocarbon types and 3 aromatic thiophenotypes in
1992)
straight run aromatic petroleum fractions boiling within the
range from 205 to 540°C (400 to 1000°F) (corrected to
3. Terminology
atmospheric pressure). Samples must be nonolefinic, must
contain not more than 1 mass% of total sulfur, and must
3.1 Definitions of Terms Specific to This Standard:
contain not more than 5% nonaromatic hydrocarbons. Com- 3.1.1 Characteristic Mass Summations— Classes I–VII:
position data are in volume percent.
3.1.2 Class I:
NOTE 1—Although names are given to 15 of the compound types
78 578192110611201.toend, polyisotopic (1)
(
determined, the presence of other compound types of the same empirical
formulae is not excluded. All other compound types in the sample,
191110511191.toend, monoisotopic
unidentified by name or empirical formula, are lumped into six groups in
accordance with their respective homologous series.
3.1.3 Class II:
1.2 The values stated in acceptable SI units are to be
104 51041118113211461.toend, polyisotopic (2)
(
regarded as the standard. The values given in parentheses are
provided for information purposes only.
1117113111451.toend, monoisotopic
1.3 This standard does not purport to address all of the
3.1.4 Class III:
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 129 51301144115811721.toend, polyisotopic (3)
(
priate safety and health practices and determine the applica-
11291143115711711.toend, monoisotopic
bility of regulatory limitations prior to use.
3.1.5 Class IV:
2. Referenced Documents
128 51281142115611701.toend, polyisotopic (4)
(
2.1 ASTM Standards:
1141115511691.toend, monoisotopic
D2549Test Method for Separation of Representative Aro-
matics and Nonaromatics Fractions of High-Boiling Oils
3.1.6 Class V:
by Elution Chromatography
154 51541168118211961.toend, polyisotopic (5)
D2786Test Method for Hydrocarbon Types Analysis of
(
1167118111951.toend, monoisotopic
1 3.1.7 Class VI:
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricantsand is the direct responsibility of
166 51661180119412081.toend, polyisotopic (6)
(
Subcommittee D02.04.0M on Mass Spectroscopy.
Current edition approved Oct. 1, 2011. Published October 2011. Originally
1179119312071.toend, monoisotopic
approved in 1973. Last previous edition approved in 2006 as D3239–91 (2006).
DOI: 10.1520/D3239-91R11.
3.1.8 Class VII:
Robinson, C. J., and Cook, G. L., Analytical Chemistry (ANCHA), Vol 41,
1969, p. 1548.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on The last approved version of this historical standard is referenced on
the ASTM website. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D3239 − 91 (2011)
6. Apparatus
178 51781192120612201.toend, polyisotopic (7)
(
6.1 Mass Spectrometer—The suitability of the mass spec-
1191120512191.toend, monoisotopic
trometer to be used with this method shall be proven by
3.1.9 Classes, Compound Types, Empirical Formulae—See
performance tests described both herein and in Practice E137.
Table 1.
6.2 Sample Inlet System—Anyinletsystemmaybeusedthat
permits the introduction of the sample without loss,
4. Summary of Test Method
contamination, or change in composition. The system must
4.1 The relative abundance of seven classes (I–VII) of
function in the range from 125 to 350°C to provide an
aromatics in petroleum aromatic fractions is determined by
appropriate sampling device.
mass spectrometry using a summation of peaks most charac-
6.3 Microburet or Constant-Volume Pipet.
teristic of each class. Calculations are carried out by the use of
6.4 Mass Spectrum Digitizer—It is recommended that a
a7by7invertedmatrixderivedfrompublishedspectraofpure
aromatic compounds. Each summation of peaks includes the mass spectrum digitizer be used in obtaining the analysis,
because it is necessary to use the heights of most of the peaks
polyisotopic homologous series that contains molecular ions
in the spectrum. Any digitizing system capable of supplying
and the monoisotopic homologous series one mass unit less
accurate mass numbers and peak heights is suitable.
than the molecular ion series. Using characteristic summations
found in the monoisotopic molecular ion—1 series of peaks,
6.5 Electronic Digital Computer—The computations for
eachclassisfurtherresolvedtoproviderelativeabundancesof
this analysis are not practical without the use of a computer.
three compound types: nominal (Type 0), first overlap (Type
Any computer capable of providing approximately 60K bytes
1), and second overlap (Type 2). The aromatic fraction is
in core and capable of compiling programs written in FOR-
obtained by liquid elution chromatography (see Test Method
TRAN IV should be suitable.
D2549).
7. Reagent
NOTE 2—Monoisotopic peaks heights are obtained by correcting the
polyisotopicheightsfornaturallyoccurringheavyisotopes,assumingthat
7.1 n-Hexadecane. (Warning—Combustible-Very harm-
only ions of C H to C H are present. This is not strictly accurate
n 2n+2 n 2−11
ful.)
for aromatics, but the errors introduced by such assumption are trivial.
5. Significance and Use 8. Calibration
8.1 Calibration equations in the computer program given in
5.1 Aknowledgeofthehydrocarboncompositionofprocess
streamsandpetroleumproductsboilingwithintherange205to Table 2 may be used directly provided the following proce-
dures are followed:
540°C (400 to 1000°F) is useful in following the effect of
changes in process variables, diagnosing the source of plant 8.1.1 Instrumental Conditions—Repeller settings are ad-
justed to maximize the m/e 226 ion of n-hexadecane. A
upsets, and in evaluating the effect of changes in composition
on product performance properties. This method, when used magnetic field is used that will permit a scan over the mass
together withTest Method D2786, provides a detailed analysis range from 78 to 700. An ionizing voltage of 70 eV and an
of the hydrocarbon composition of such materials. ionizing current in the range from 10 to 70 µA is used.
NOTE3—Theinstrumentconditionsandcalibrationequationsdescribed
in this method are based on the use of a 180° magnetic-deflection type
TABLE 1 Classes, Compound Types, and Empirical Formulae
mass spectrometer (CEC Model 21-103). Satisfactory results have been
Class Type Formula
obtainedwithsomeothermagneticdeflectioninstruments.Itisnotknown
I 0 alkylbenzenes, C H
n 2n-6
if the equations are suitable for use on all other mass spectrometer types.
I 1 benzothiophenes, C H S
n 2n-10
8.1.2 Computer Program—The FORTRAN program given
I 2 naphthenephenanthrenes,
C H
n 2n-20
in Table 2 contains all the equations for calculating the
II 0 naphthenebenzenes, C H
...

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5.1 The basic test method of determining the boiling range of a petroleum product by performing a simple batch distillation has been in use as long as the petroleum industry has existed. It is one of the oldest test methods under the jurisdiction of ASTM Committee D02, dating from the time when it was still referred to as the Engler distillation. Since the test method has been in use for such an extended period, a tremendous number of historical data bases exist for estimating end-use sensitivity on products and processes.  
5.2 The distillation (volatility) characteristics of hydrocarbons have an important effect on their safety and performance, especially in the case of fuels and solvents. The boiling range gives information on the composition, the properties, and the behavior of the fuel during storage and use. Volatility is the major determinant of the tendency of a hydrocarbon mixture to produce potentially explosive vapors.  
5.3 The distillation characteristics are critically important for both automotive and aviation gasolines, affecting starting, warm-up, and tendency to vapor lock at high operating temperature or at high altitude, or both. The presence of high boiling point components in these and other fuels can significantly affect the degree of formation of solid combustion deposits.  
5.4 Volatility, as it affects rate of evaporation, is an important factor in the application of many solvents, particularly those used in paints.  
5.5 Distillation limits are often included in petroleum product specifications, in commercial contract agreements, process refinery/control applications, and for compliance to regulatory rules.
SCOPE
1.1 This test method covers the atmospheric distillation of petroleum products and liquid fuels using a laboratory batch distillation unit to determine quantitatively the boiling range characteristics of such products as light and middle distillates, automotive spark-ignition engine fuels with or without oxygenates (see Note 1), aviation gasolines, aviation turbine fuels, diesel fuels, biodiesel blends up to 30 % volume, marine fuels, special petroleum spirits, naphthas, white spirits, kerosines, and Grades 1 and 2 burner fuels.
Note 1: An interlaboratory study was conducted in 2008 involving 11 different laboratories submitting 15 data sets and 15 different samples of ethanol-fuel blends containing 25 % volume, 50 % volume, and 75 % volume ethanol. The results indicate that the repeatability limits of these samples are comparable or within the published repeatability of the method (with the exception of FBP of 75 % ethanol-fuel blends). On this basis, it can be concluded that Test Method D86 is applicable to ethanol-fuel blends such as Ed75 and Ed85 (Specification D5798) or other ethanol-fuel blends with greater than 10 % volume ethanol. See ASTM RR:D02-1694 for supporting data.2  
1.2 The test method is designed for the analysis of distillate fuels; it is not applicable to products containing appreciable quantities of residual material.  
1.3 This test method covers both manual and automated instruments.  
1.4 Unless otherwise noted, the values stated in SI units are to be regarded as the standard. The values given in parentheses are provided for information only.  
1.5 WARNING—Mercury has been designated by many regulatory agencies as a hazardous substance that can cause serious medical issues. Mercury, or its vapor, has been demonstrated to be hazardous to health and corrosive to materials. Use Caution when handling mercury and mercury-containing products. See the applicable product Safety Data Sheet (SDS) for additional information. The potential exists that selling mercury or mercury-containing products, or both, is prohibited by local or national law. Users must determine legality of sales in their location.  
1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilit...

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ASTM
ASTM D2425-23(Test Method)
Standard Test Method for Hydrocarbon Types in Middle Distillates by Mass Spectrometry

SIGNIFICANCE AND USE
5.1 A knowledge of the hydrocarbon composition of process streams and petroleum products boiling within the range of 160 °C to 343 °C (320 °F to 650 °F) is useful in following the effect of changes in process variables, diagnosing the source of plant upsets, and in evaluating the effect of changes in composition on product performance properties.  
5.2 A test method to determine total cycloparafins and low level aromatic content is necessary to meet specifications for aviation turbine fuel containing synthesized hydrocarbons.
SCOPE
1.1 This test method covers an analytical scheme using the mass spectrometer to determine the hydrocarbon types present in conventional and synthesized hydrocarbons that have a boiling range of 160 °C to 343 °C (320 °F to 650 °F), 5 % to 95 % by volume as determined by Test Method D86. Samples with average carbon number value of paraffins between C12 and C16 and containing paraffins from C10 and C18 can be analyzed. Eleven hydrocarbon types are determined. These include: paraffins, noncondensed cycloparaffins, condensed dicycloparaffins, condensed tricycloparaffins, alkylbenzenes, indans or tetralins, or both, CnH 2n-10 (indenes, etc.), naphthalenes, CnH2n-14  (acenaphthenes, etc.), CnH 2n-16 (acenaphthylenes, etc.), and tricyclic aromatics.  
Note 1: This test method was developed on Consolidated Electrodynamics Corporation Type 103 Mass Spectrometers. Operating parameters for users with a Quadrupole Mass Spectrometer are provided.  
1.2 This test method is intended for use with full boiling range products that contain no significant olefin content.
Biodiesel (FAME components) could interfere with the separation of the sample and the characteristic mass fragments of FAME compounds are not defined in the procedure.
Hydrocarbons containing tertiary carbon fragments, sometimes found in synthetic aviation fuels, will interfere with the characteristic mass fragments of paraffins and result in a false, elevated cycloparaffin content.
Note 2: “No significant olefin content” for this method means D1319.  
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. For a specific warning statement, see 11.1.  
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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ASTM
ASTM D665-23(Test Method)
Standard Test Method for Rust-Preventing Characteristics of Inhibited Mineral Oil in the Presence of Water

SIGNIFICANCE AND USE
5.1 In many instances, such as in the gears of a steam turbine, water can become mixed with the lubricant, and rusting of ferrous parts can occur. This test indicates how well inhibited mineral oils aid in preventing this type of rusting. This test method is also used for testing hydraulic and circulating oils, including heavier-than-water fluids. It is used for specification of new oils and monitoring of in-service oils.
Note 3: This test method was used as a basis for Test Method D3603. Test Method D3603 is used to test the oil on separate horizontal and vertical test rod surfaces, and can provide a more discriminating evaluation.
SCOPE
1.1 This test method covers the evaluation of the ability of inhibited mineral oils, particularly steam-turbine oils, to aid in preventing the rusting of ferrous parts should water become mixed with the oil. This test method is also used for testing other oils, such as hydraulic oils and circulating oils. Provision is made in the procedure for testing heavier-than-water fluids.
Note 1: For synthetic fluids, such as phosphate ester types, the plastic holder and beaker cover should be made of chemically resistant material suitable for the type of fluid tested.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific warning statements, see 7.4 – 7.6.  
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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