ASTM D4045-04

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Designation:D4045–04
Standard Test Method for
Sulfur in Petroleum Products by Hydrogenolysis and
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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
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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. ,
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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
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D6299 Practice for Applying Statistical Quality Assurance
contain H S in proportion to sulfur in the sample. The HSis
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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).
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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.)
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This test method is under the jurisdiction of ASTM Committee D02 on
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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.
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10.1520/D4045-04. The sole source of supply of the apparatus known to the committee at this time
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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
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Standards volume information, refer
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