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ASTM D4294-02

(Test Method)

Standard Test Method for Sulfur in Petroleum Products by Energy-Dispersive X-Ray Fluorescence Spectroscopy

Standard Test Method for Sulfur in Petroleum Products by Energy-Dispersive X-Ray Fluorescence Spectroscopy

SCOPE
1.1 This test method covers the measurement of sulfur in hydrocarbons, such as diesel, naphtha, kerosine, residuals, lubricating base oils, hydraulic oils, jet fuels, crude oils, gasoline (all unleaded), and other distillates. In addition, sulfur in other products, such as M-85 and M-100, may be analyzed using this technique. The applicable concentration range is 0.0150 to 5.00 mass % sulfur.
1.2 The values stated in SI units are to be regarded as the standard. The preferred concentration units are mass % sulfur.
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. For specific warning statements, see Section 7.

General Information

Status
Historical
Publication Date
09-Apr-2002
ICS
75.080 - Petroleum products in general
Technical Committee
D02 - Petroleum Products, Liquid Fuels, and Lubricants
Current Stage
Ref Project

Relations

Replaced By
ASTM D4294-03 - Standard Test Method for Sulfur in Petroleum and Petroleum Products by Energy-Dispersive X-Ray Fluorescence Spectrometry
Effective Date
01-Nov-2003
Referred By
ASTM D7156-19 - Standard Test Method for Evaluation of Diesel Engine Oils in the T-11 Exhaust Gas Recirculation Diesel Engine
Effective Date
10-Apr-2002
Referred By
ASTM D7547-23 - Standard Specification for Hydrocarbon Unleaded Aviation Gasoline
Effective Date
10-Apr-2002
Referred By
ASTM D2880-23 - Standard Specification for Gas Turbine Fuel Oils
Effective Date
10-Apr-2002
Referred By
ASTM D8434-21 - Standard Specification for Unleaded Aviation Gasoline Test Fuel Containing Organo-metallic Additive
Effective Date
10-Apr-2002
Referred By
ASTM D7578-20 - Standard Guide for Calibration Requirements for Elemental Analysis of Petroleum Products and Lubricants
Effective Date
10-Apr-2002
Referred By
ASTM D6823-08(2021) - Standard Specification for Commercial Boiler Fuels With Used Lubricating Oils
Effective Date
10-Apr-2002
Referred By
ASTM D1655-23 - Standard Specification for Aviation Turbine Fuels
Effective Date
10-Apr-2002
Referred By
ASTM D8056-18 - Standard Guide for Elemental Analysis of Crude Oil
Effective Date
10-Apr-2002
Referred By
ASTM D6615-22 - Standard Specification for Jet B Wide-Cut Aviation Turbine Fuel
Effective Date
10-Apr-2002
Referred By
ASTM D396-21 - Standard Specification for Fuel Oils
Effective Date
10-Apr-2002
Referred By
ASTM D3338/D3338M-20a - Standard Test Method for Estimation of Net Heat of Combustion of Aviation Fuels
Effective Date
10-Apr-2002
Referred By
ASTM D8147-17(2023) - Standard Specification for Special-Purpose Test Fuels for Aviation Compression-Ignition Engines
Effective Date
10-Apr-2002
Referred By
ASTM D6709-22 - Standard Test Method for Evaluation of Automotive Engine Oils in the Sequence VIII Spark-Ignition Engine (CLR Oil Test Engine)
Effective Date
10-Apr-2002
Referred By
ASTM D7468-22 - Standard Test Method for Cummins ISM Test
Effective Date
10-Apr-2002

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ASTM D4294-02 - Standard Test Method for Sulfur in Petroleum Products by Energy-Dispersive X-Ray Fluorescence SpectroscopyASTM D4294-02 - Standard Test Method for Sulfur in Petroleum Products by Energy-Dispersive X-Ray Fluorescence Spectroscopy
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ASTM D4294-02 - Standard Test Method for Sulfur in Petroleum Products by Energy-Dispersive X-Ray Fluorescence Spectroscopy
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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
An American National Standard
Designation: D 4294 – 02
Standard Test Method for
Sulfur in Petroleum and Petroleum Products by Energy-
1
Dispersive X-ray Fluorescence Spectrometry
This standard is issued under the fixed designation D 4294; 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 (e) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope from previously prepared calibration standards that bracket the
sample concentration range of interest to obtain the sulfur
1.1 This test method covers the measurement of sulfur in
concentration in mass %.
hydrocarbons, such as diesel, naphtha, kerosine, residuals,
lubricating base oils, hydraulic oils, jet fuels, crude oils,
4. Significance and Use
gasoline (all unleaded), and other distillates. In addition, sulfur
4.1 This test method provides rapid and precise measure-
in other products, such as M-85 and M-100, may be analyzed
ment of total sulfur in petroleum products with a minimum of
using this technique. The applicable concentration range is
sample preparation. A typical analysis time is 2 to 4 min per
0.0150 to 5.00 mass % sulfur.
sample.
1.2 The values stated in SI units are to be regarded as the
4.2 The quality of many petroleum products is related to the
standard. The preferred concentration units are mass % sulfur.
amount of sulfur present. Knowledge of sulfur concentration is
1.3 This standard does not purport to address all of the
necessary for processing purposes. There are also regulations
safety concerns, if any, associated with its use. It is the
promulgated in federal, state, and local agencies that restrict
responsibility of the user of this standard to establish appro-
the amount of sulfur present in some fuels.
priate safety and health practices and determine the applica-
4.3 This test method provides a means of compliance with
bility of regulatory limitations prior to use. For specific
specifications or limits set by regulations for sulfur content of
warning statements, see Section 7.
petroleum products.
2. Referenced Documents 4.4 If this test method is applied to petroleum matrices with
significantly different composition than the white oil calibra-
2.1 ASTM Standards:
tion materials specified in this test method, the cautions and
D 3120 Test Method for Trace Quantities of Sulfur in Light
recommendations in Section 5 should be observed when
Liquid Petroleum Hydrocarbons by Oxidative Microcou-
2 interpreting the results.
lometry
4.5 Compared to other test methods for sulfur determina-
D 4057 Practice for Manual Sampling of Petroleum and
3 tion, Test Method D 4294 has high throughput, minimal sample
Petroleum Products
preparation, good precision, and is capable of determining
D 4177 Practice for Automatic Sampling of Petroleum and
3 sulfur over a wide range of concentrations. The equipment
Petroleum Products
specified is in most cases less costly than that required for
E 29 Practice for Using Significant Digits in Test Data to
5
4 alternative methods. Consult the ASTM Subject Index for
Determine Conformance with Specifications
names of alternative test methods.
3. Summary of Test Method
5. Interferences
3.1 The sample is placed in the beam emitted from an X-ray
5.1 Spectral interferences result when some sample compo-
source. The resultant excited characteristic X radiation is
nent element or elements emit X-rays that the detector cannot
measured, and the accumulated count is compared with counts
resolve from sulfur X-ray emission. As a result, the lines
produce spectral peaks that overlap with each other. Spectral
interferences may arise from samples containing water, lead
1
This test method is under the jurisdiction of Committee D02 on Petroleum
alkyls, silicon, phosphorus, calcium, potassium, and halides if
Products and Lubricants and is the direct responsibility of Subcommittee D02.03 on
present at concentrations greater than one tenth of the mea-
Elemental Analysis.
sured concentration of sulfur, or more than a few hundred
Current edition approved April 10, 2002. Published July 2002. Originally
published as D 4294-83. Last previous edition D 4294-98.
2
Annual Book of ASTM Standards, Vol 05.01.
3
Annual Book of ASTM Standards, Vol 05.02.
4 5
Annual Book of ASTM Standards, Vol 14.02. Annual Book of ASTM Standards, Vol 00.01.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
D4294–02
milligrams/kilogram. Follow the manufacturer’s operating- 6.1.3 X-ray Detector, with sensitivity at 2.3
...

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5.1 The boiling range distribution of light and medium petroleum distillate fractions provides an insight into the composition of feed stocks and products related to petroleum refining process, This gas chromatographic determination of boiling range 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.  
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Standard Test Method for Bromine Numbers of Petroleum Distillates and Commercial Aliphatic Olefins by Electrometric Titration

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5.1 The bromine number is useful as a measure of aliphatic unsaturation in petroleum samples. When used in conjunction with the calculation procedure described in Annex A2, it can be used to estimate the percentage of olefins in petroleum distillates boiling up to approximately 315 °C (600 °F).  
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1.5 WARNING—Mercury has been designated by many regulatory agencies as a hazardous substance that can cause serious medical issues. Mercury, or its vapor, has been demonstrated to be hazardous to health and corrosive to materials. Use Caution when handling mercury and mercury-containing products. See the applicable product Safety Data Sheet (SDS) for additional information. The potential exists that selling mercury or mercury-containing products, or both, is prohibited by local or national law. Users must determine legality of sales in their location.  
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1.1 This test method covers the determination of solvent extractables in petroleum waxes.  
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5.1 Determination of the color of petroleum products is used mainly for manufacturing control purposes and is an important quality characteristic since color is readily observed by the user of the product. In some cases the color may serve as an indication of the degree of refinement of the material. When the color range of a particular product is known, a variation outside the established range can indicate possible contamination with another product. However, color is not always a reliable guide to product quality and should not be used indiscriminately in product specifications.
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Note 1: For determining the color of petroleum products darker than Saybolt Color − 16, see Test Method D1500.  
1.2 This test method reports results specific to this test method and recorded as, “Saybolt Color units.”  
1.3 The values stated in inch-pound units or in SI units and which are not in parentheses are to be regarded as the standard. The values given in parentheses are for information only.  
Note 2: Oil tubes and apparatus used in this test method have traditionally been marked in inches, (the tube is required to be etched with 1/8 in. divisions.) The Saybolt Color Numbers are aligned with inch, 1/2 in., 1/4 in., and 1/8 in. changes in the depth of oil. These fractional inch changes do not readily correspond to SI equivalents and in view of the preponderance of apparatus already in use and marked in inches, the inch/pound unit is regarded as the standard. However the test method does use SI units of length when the length is not directly related to divisions on the oil tube and Saybolt Color Numbers. The test method uses SI units for temperature.  
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Standard Practice for Calculating Viscosity of a Blend of Petroleum Products

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5.1 Predicting the viscosity of a blend of components is a common problem. Both the Wright Blending Method and the ASTM Blending Method, described in this practice, may be used to solve this problem.  
5.2 The inverse problem, predicating the required blend fractions of components to meet a specified viscosity at a given temperature may also be solved using either the Inverse Wright Blending Method or the Inverse ASTM Blending Method.  
5.3 The Wright Blending Methods are generally preferred since they have a firmer basis in theory, and are more accurate. The Wright Blending Methods require component viscosities to be known at two temperatures. The ASTM Blending Methods are mathematically simpler and may be used when viscosities are known at a single temperature.  
5.4 Although this practice was developed using kinematic viscosity and volume fraction of each component, the dynamic viscosity or mass fraction, or both, may be used instead with minimal error if the densities of the components do not differ greatly. For fuel blends, it was found that viscosity blending using mass fractions gave more accurate results. For base stock blends, there was no significant difference between mass fraction and volume fraction calculations.  
5.5 The calculations described in this practice have been computerized as a spreadsheet and are available as an adjunct.3
SCOPE
1.1 This practice covers the procedures for calculating the estimated kinematic viscosity of a blend of two or more petroleum products, such as lubricating oil base stocks, fuel components, residual fuel oil with kerosene, crude oils, and related products, from their kinematic viscosities and blend fractions.  
1.2 This practice allows for the estimation of the fraction of each of two petroleum products needed to prepare a blend meeting a specific viscosity.  
1.3 This practice may not be applicable to other types of products, or to materials which exhibit strong non-Newtonian properties, such as viscosity index improvers, additive packages, and products containing particulates.  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.5 Logarithms may be either common logarithms or natural logarithms, as long as the same are used consistently. This practice uses common logarithms. If natural logarithms are used, the inverse function, exp(×), must be used in place of the base 10 exponential function, 10×, used herein.  
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ASTM D4952-23(Test Method)
Standard Test Method for Qualitative Analysis for Active Sulfur Species in Fuels and Solvents (Doctor Test)

SIGNIFICANCE AND USE
5.1 Sulfur present as mercaptans or as hydrogen sulfide in distillate fuels and solvents can attack many metallic and non-metallic materials in fuel and other distribution systems. A negative result in the doctor test ensures that the concentration of these compounds is insufficient to cause such problems in normal use.
SCOPE
1.1 This test method covers and is intended primarily for the detection of mercaptans in motor fuel, kerosine, and similar petroleum products. This method may also provide information on hydrogen sulfide and elemental sulfur that may be present in these sample types.  
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 7.3.  
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ASTM D2887-23(Test Method)
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.

  • Standard
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  • Standard
    35 pages
    English language
    sale 15% off