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ASTM D4045-04

(Test Method)

Standard Test Method for Sulfur in Petroleum Products by Hydrogenolysis and Rateometric Colorimetry

Standard Test Method for Sulfur in Petroleum Products by Hydrogenolysis and Rateometric Colorimetry

SIGNIFICANCE AND USE
In many petroleum refining processes, low levels of sulfur in feed stocks may poison expensive catalysts. This test method can be used to monitor the amount of sulfur in such petroleum fractions.
This test method may also be used as a quality-control tool for sulfur determination in finished products.
SCOPE
1.1 This test method covers the determination of sulfur in petroleum products in the range from 0.02 to 10.00 mg/kg.
1.2 This test method may be extended to higher concentration by dilution.
1.3 This test method is applicable to liquids whose boiling points are between 30 and 371°C (86 and 700°F). Materials that can be analyzed include naphtha, kerosine, alcohol, steam condensate, various distillates, jet fuel, benzene, and toluene.
1.4 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.4.1 Certain specifications for the recorder (see 5.5) are excepted.
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

General Information

Status
Historical
Publication Date
30-Apr-2004
ICS
75.080 - Petroleum products in general
Technical Committee
D02 - Petroleum Products, Liquid Fuels, and Lubricants
Drafting Committee
D02.03 - Elemental Analysis
Current Stage
Ref Project

Relations

Replaces
ASTM D4045-99 - Standard Test Method for Sulfur in Petroleum Products by Hydrogenolysis and Rateometric Colorimetry
Effective Date
01-May-2004
Replaced By
ASTM D4045-04(2010) - Standard Test Method for Sulfur in Petroleum Products by Hydrogenolysis and Rateometric Colorimetry
Effective Date
01-May-2010
Referred By
ASTM D7578-20 - Standard Guide for Calibration Requirements for Elemental Analysis of Petroleum Products and Lubricants
Effective Date
01-May-2004
Referred By
ASTM D5983-21 - Standard Specification for Methyl Tertiary-Butyl Ether (MTBE) for Blending With Gasolines for Use as Automotive Spark-Ignition Engine Fuel
Effective Date
01-May-2004
Referred By
ASTM D7212-13(2018) - Standard Test Method for Low Sulfur in Automotive Fuels by Energy-Dispersive X-ray Fluorescence Spectrometry Using a Low-Background Proportional Counter
Effective Date
01-May-2004
Referred By
ASTM D7455-19 - Standard Practice for Sample Preparation of Petroleum and Lubricant Products for Elemental Analysis
Effective Date
01-May-2004
Referred By
ASTM D4468-23 - Standard Test Method for Total Sulfur in Gaseous Fuels by Hydrogenolysis and<brk/> Rateometric Colorimetry
Effective Date
01-May-2004

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ASTM D4045-04 - Standard Test Method for Sulfur in Petroleum Products by Hydrogenolysis and Rateometric ColorimetryASTM D4045-04 - Standard Test Method for Sulfur in Petroleum Products by Hydrogenolysis and Rateometric Colorimetry
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ASTM D4045-04 - Standard Test Method for Sulfur in Petroleum Products by Hydrogenolysis and Rateometric Colorimetry
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Standards Content (Sample)

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:D4045–04
Standard Test Method for
Sulfur in Petroleum Products by Hydrogenolysis and
1
Rateometric Colorimetry
This standard is issued under the fixed designation D4045; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope* reactionofH Swithleadacetate.Condensablecomponentsare
2
converted to gaseous products, such as methane, during hydro-
1.1 This test method covers the determination of sulfur in
genolysis.
petroleum products in the range from 0.02 to 10.00 mg/kg.
1.2 This test method may be extended to higher concentra-
4. Significance and Use
tion by dilution.
4.1 In many petroleum refining processes, low levels of
1.3 This test method is applicable to liquids whose boiling
sulfur in feed stocks may poison expensive catalysts. This test
points are between 30 and 371°C (86 and 700°F). Materials
method can be used to monitor the amount of sulfur in such
that can be analyzed include naphtha, kerosine, alcohol, steam
petroleum fractions.
condensate, various distillates, jet fuel, benzene, and toluene.
4.2 This test method may also be used as a quality-control
1.4 The values stated in SI units are to be regarded as
tool for sulfur determination in finished products.
standard. The values given in parentheses are for information
only. ,
34
5. Apparatus
1.4.1 Certain specifications for the recorder (see 5.5) are
5.1 Pyrolysis Furnace—A furnace that can provide an
excepted.
adjustable temperature from 900 to 1400°C in a 5-mm inside
1.5 This standard does not purport to address all of the
diameter or larger tube is required to pyrolyze the sample. The
safety concerns, if any, associated with its use. It is the
furnace entry temperature shall allow insertion of the hypoder-
responsibility of the user of this standard to establish appro-
mic tip to a depth at which the temperature is 550°C to provide
priate safety and health practices and determine the applica-
sample vaporization at the injection syringe tip. This tempera-
bility of regulatory limitations prior to use.
ture shall be above the boiling point of the sample and of the
2. Referenced Documents sulfur compounds in the sample (see Fig. 1). The pyrolyzer
2 tube may be of quartz; however, the lifetime is limited above
2.1 ASTM Standards:
1250°C. Ceramic may be used at any temperature.
D1193 Specification for Reagent Water
5.2 Rateometric H S Readout— Hydrogenolysis products
2
D6299 Practice for Applying Statistical Quality Assurance
contain H S in proportion to sulfur in the sample. The HSis
2 2
and Control Charting Techniques to Evaluate Analytical
measuredbymeasuringrateofchangeofreflectancecausedby
Measurement System Performance
darkening when lead sulfide is formed. Rateometric electron-
3. Summary of Test Method ics, adapted to provide a first derivative output, allows suffi-
cient sensitivity to measure below 0.1 mg/L (see Fig. 2).
3.1 The sample is injected at a constant rate into a flowing
5.3 Hypodermic Syringe—A hypodermic having a needle
hydrogen stream in a hydrogenolysis apparatus. The sample
long enough to reach the 550°C zone is required.Aside port is
and hydrogen are pyrolyzed at a temperature of 1300°C, or
convenient for vacuum filling and for flushing the syringe. A
above, to convert sulfur compounds to hydrogen sulfide (H S).
2
100-µL syringe is satisfactory for injection rates down to 3
Readout is by the rateometric detection of the colorimetric
µL/min and a 25-µL syringe for lower rates. (Warning—
Exercise caution as hypodermics can cause accidental injury.)
1
This test method is under the jurisdiction of ASTM Committee D02 on
3
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee The apparatus described in 5.1-5.4 inclusive is similar in specification to the
D02.03 on Elemental Analysis. equipment available from Houston Atlas, Inc., 22001 North Park Dr., Kingswood,
Current edition approved May 1, 2004. Published June 2004. Originally TX 77339-3804. For further information see Drushel, H. V., “Trace Sulfur
approved in 1987. Last previous edition approved in 1999 as D4045–99. DOI: Determination Petroleum Fractions,” Analytical Chemistry, Vol 50, 1978, p. 76.
4
10.1520/D4045-04. The sole source of supply of the apparatus known to the committee at this time
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or is Houston Atlas, Inc. If you are aware of alternative suppliers, please provide this
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM information to ASTM International Headquarters. Your comments will receive
1
Standards volume information, refer
...

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Standard Test Method for Bromine Numbers of Petroleum Distillates and Commercial Aliphatic Olefins by Electrometric Titration

SIGNIFICANCE AND USE
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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1.1 This test method3 covers the determination of the bromine number of the following materials:  
1.1.1 Petroleum distillates that are substantially free of material lighter than isobutane and that have 90 % distillation points (by Test Method D86) under 327 °C (626 °F). This test method is generally applicable to gasoline (including leaded, unleaded, and oxygenated fuels), kerosine, and distillates in the gas oil range that fall in the following limits:    
90 % Distillation Point, °C (°F)  
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Note 1: These limits are imposed since the precision of this test method has been determined only up to or within the range of these bromine numbers.  
1.2 The magnitude of the bromine number is an indication of the quantity of bromine-reactive constituents, not an identification of constituents; therefore, its application as a measure of olefinic unsaturation should not be undertaken without the study given in Annex A1.  
1.3 For petroleum hydrocarbon mixtures of bromine number less than 1.0, a more precise measure for bromine-reactive constituents can be obtained by using Test Method D2710. If the bromine number is less than 0.5, then Test Method D2710 or the comparable bromine index methods for industrial aromatic hydrocarbons, Test Methods D1492 or D5776 must be used in accordance with their respective scopes. The practice of using a factor of 1000 to convert bromine number to bromine index is not applicable for these lower values of bromine number.  
1.4 The values stated in SI units are to be regarded as the standard.  
1.4.1 Exception—The values given in parentheses are for information only.  
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ASTM D7213-23(Test Method)
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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.  
5.2 This test method extends the scope of boiling range determination by gas chromatography to include light and medium petroleum distillate fractions beyond the scope of Test Method D2887 (538 °C) and below Test Method D6352 (700 °C).  
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SCOPE
1.1 This test method covers the determination of the boiling range distribution of petroleum products. This test method is applicable to petroleum distillates having an initial boiling point greater than 100 °C and a final boiling point less than 615 °C at atmospheric pressure as measured by this test method.  
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ASTM D2890-23(Test Method)
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SIGNIFICANCE AND USE
5.1 Heat capacities obtained by this method are those at atmospheric pressure. However, because the temperature range is low, the calculated values are similar to saturated liquid heat capacities in the temperature-pressure range required for most engineering design.
SCOPE
1.1 This test method covers the calculation of liquid heat capacity, Btu/lb · °F (kJ/kg · K), at atmospheric pressure, of petroleum fuels for which distillation data may be obtained in accordance with Test Method D86 without reaching a decomposition point prior to obtaining 90 % by volume distilled.  
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5.1 The solvent extractables in a wax may have significant effects on several of its properties such as strength, hardness, flexibility, scuff resistance, coefficient of friction, coefficient of expansion, melting point, and staining characteristics. Whether these effects are desirable or undesirable depends on the intended use of the wax.
SCOPE
1.1 This test method covers the determination of solvent extractables in petroleum waxes.  
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1.1 This test method covers the determination of the color of refined oils such as undyed motor and aviation gasoline, jet propulsion fuels, naphthas and kerosine, and, in addition, petroleum waxes and pharmaceutical white oils.  
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 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.

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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.  
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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  • Standard
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