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ASTM D4045-99

(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

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 The method may be extended to higher concentration by dilution.  
1.3 The method is applicable to liquids whose boiling points are between 30 to 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 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
09-Jan-1999
ICS
75.080 - Petroleum products in general
Technical Committee
D02 - Petroleum Products, Liquid Fuels, and Lubricants
Current Stage
Ref Project

Relations

Replaced By
ASTM D4045-04 - Standard Test Method for Sulfur in Petroleum Products by Hydrogenolysis and Rateometric Colorimetry
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
10-Jan-1999
Referred By
ASTM D7455-19 - Standard Practice for Sample Preparation of Petroleum and Lubricant Products for Elemental Analysis
Effective Date
10-Jan-1999
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
10-Jan-1999
Referred By
ASTM D7578-20 - Standard Guide for Calibration Requirements for Elemental Analysis of Petroleum Products and Lubricants
Effective Date
10-Jan-1999
Referred By
ASTM D4468-23 - Standard Test Method for Total Sulfur in Gaseous Fuels by Hydrogenolysis and<brk/> Rateometric Colorimetry
Effective Date
10-Jan-1999

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ASTM D4045-99 - Standard Test Method for Sulfur in Petroleum Products by Hydrogenolysis and Rateometric ColorimetryASTM D4045-99 - Standard Test Method for Sulfur in Petroleum Products by Hydrogenolysis and Rateometric Colorimetry
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ASTM D4045-99 - 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
An American National Standard
Designation: D 4045 – 99
Standard Test Method for
Sulfur in Petroleum Products by Hydrogenolysis and
1
Rateometric Colorimetry
This standard is issued under the fixed designation D 4045; 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.
1. Scope 4. Significance and Use
4.1 In many petroleum refining processes, low levels of
1.1 This test method covers the determination of sulfur in
petroleum products in the range from 0.02 to 10.00 mg/kg. sulfur in feed stocks may poison expensive catalysts. This test
1.2 The method may be extended to higher concentration by method can be used to monitor the amount of sulfur in such
dilution. petroleum fractions.
1.3 The method is applicable to liquids whose boiling points 4.2 This test method may also be used as a quality-control
are between 30 and 371°C (86 and 700°F). Materials that can tool for sulfur determination in finished products.
be analyzed include naphtha, kerosine, alcohol, steam conden-
,
4 5
5. Apparatus
sate, various distillates, jet fuel, benzene, and toluene.
1.4 The values in acceptable SI units are to be regarded as 5.1 Pyrolysis Furnace—A furnace that can provide an
adjustable temperature from 900 to 1400°C in a 5-mm inside
the standard. The values in parentheses are for information
only. diameter or larger tube is required to pyrolyze the sample. The
furnace entry temperature shall allow insertion of the hypoder-
1.4.1 Certain specifications for the recorder (see 5.5) are
excepted. mic tip to a depth at which the temperature is 550°C to provide
sample vaporization at the injection syringe tip. This tempera-
1.5 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the ture shall be above the boiling point of the sample and of the
sulfur compounds in the sample (see Fig. 1). The pyrolyzer
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- tube may be of quartz; however, the lifetime is limited above
1250°C. Ceramic may be used at any temperature.
bility of regulatory limitations prior to use.
5.2 Rateometric H S Readout— Hydrogenolysis products
2
2. Referenced Documents
contain H S in proportion to sulfur in the sample. The H Sis
2 2
2.1 ASTM Standards: measured by measuring rate of change of reflectance caused by
2
D 1193 Specification for Reagent Water darkening when lead sulfide is formed. Rateometric electron-
D 6299 Practice for Applying Statisitical Quality Assurance ics, adapted to provide a first derivative output, allows suffi-
Techniques to Evaluate Analytical Measurement System cient sensitivity to measure below 0.1 mg/L (see Fig. 2).
3
Performance 5.3 Hypodermic Syringe—A hypodermic having a needle
long enough to reach the 550°C zone is required. A side port is
3. Summary of Test Method
convenient for vacuum filling and for flushing the syringe.
3.1 The sample is injected at a constant rate into a flowing
A100-μL syringe is satisfactory for injection rates down to 3
hydrogen stream in a hydrogenolysis apparatus. The sample μL/min and a 25-μL syringe for lower rates.
and hydrogen are pyrolyzed at a temperature of 1300°C, or
NOTE 1—Warning: Exercise caution as hypodermics can cause acci-
above, to convert sulfur compounds to hydrogen sulfide (H S).
2
dental injury.
Readout is by the rateometric detection of the colorimetric
5.4 Syringe Injection Drive—The drive shall provide uni-
reaction of H S with lead acetate. Condensable components are
2
form, continuous sample injections. Variation in drive injection
converted to gaseous products, such as methane, during hydro-
genolysis.
4
The apparatus described in 5.1-5.4 inclusive is similar in specification to the
1
This test method is under the jurisdiction of ASTM Committee D-2 on equipment available from Houston Atlas, Inc., 22001 North Park Dr., Kingswood,
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee TX 77339-3804. For further information see Drushel, H. V., “Trace Sulfur
D02.03 on Elemental Analysis. Determination Petroleum Fractions,” Analytical Chemistry, Vol 50, 1978, p. 76.
5
Current edition approved Jan. 10, 1999. Published March 1999. Originally Houston Atlas, Inc. is the sole source of supply of the apparatus known to the
published as D 4045 – 87. Last previous edition D 4045 – 96. committee at this time. If you are aware of alternative suppliers, please provide this
2
Annual Book of ASTM Standards, Vol 11.01. information to ASTM Headquarters. Your comments will receive careful consider-
3 1
Annual
...

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

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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.  
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