ASTM D4045-04(2010)
(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 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
Relations
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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(Reapproved 2010)
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 above, to convert sulfur compounds to hydrogen sulfide (H S).
2
Readout is by the rateometric detection of the colorimetric
1.1 This test method covers the determination of sulfur in
reactionofH Swithleadacetate.Condensablecomponentsare
2
petroleum products in the range from 0.02 to 10.00 mg/kg.
converted to gaseous products, such as methane, during hy-
1.2 This test method may be extended to higher concentra-
drogenolysis.
tion by dilution.
4. Significance and Use
1.3 This test method is applicable to liquids whose boiling
points are between 30 and 371°C (86 and 700°F). Materials 4.1 In many petroleum refining processes, low levels of
that can be analyzed include naphtha, kerosine, alcohol, steam
sulfur in feed stocks may poison expensive catalysts. This test
condensate, various distillates, jet fuel, benzene, and toluene. method can be used to monitor the amount of sulfur in such
petroleum fractions.
1.4 The values stated in SI units are to be regarded as
standard. The values given in parentheses are for information 4.2 This test method may also be used as a quality-control
only.
tool for sulfur determination in finished products.
1.4.1 Certain specifications for the recorder (see 5.5) are
3,4
5. Apparatus
excepted.
5.1 Pyrolysis Furnace—A furnace that can provide an
1.5 This standard does not purport to address all of the
adjustable temperature from 900 to 1400°C in a 5-mm inside
safety concerns, if any, associated with its use. It is the
diameter or larger tube is required to pyrolyze the sample. The
responsibility of the user of this standard to establish appro-
furnace entry temperature shall allow insertion of the hypoder-
priate safety and health practices and determine the applica-
mic tip to a depth at which the temperature is 550°C to provide
bility of regulatory limitations prior to use.
sample vaporization at the injection syringe tip. This tempera-
2. Referenced Documents ture shall be above the boiling point of the sample and of the
2 sulfur compounds in the sample (see Fig. 1). The pyrolyzer
2.1 ASTM Standards:
tube may be of quartz; however, the lifetime is limited above
D1193 Specification for Reagent Water
1250°C. Ceramic may be used at any temperature.
D6299 Practice for Applying Statistical Quality Assurance
and Control Charting Techniques to Evaluate Analytical 5.2 Rateometric H S Readout— Hydrogenolysis products
2
Measurement System Performance contain H S in proportion to sulfur in the sample. The HSis
2 2
measuredbymeasuringrateofchangeofreflectancecausedby
3. Summary of Test Method
darkening when lead sulfide is formed. Rateometric
electronics, adapted to provide a first derivative output, allows
3.1 The sample is injected at a constant rate into a flowing
sufficient sensitivity to measure below 0.1 mg/L (see Fig. 2).
hydrogen stream in a hydrogenolysis apparatus. The sample
and hydrogen are pyrolyzed at a temperature of 1300°C, or
5.3 Hypodermic Syringe—A hypodermic having a needle
long enough to reach the 550°C zone is required.Aside port is
1
This test method is under the jurisdiction of ASTM Committee D02 on
3
Petroleum Products, Liquid Fuels, and Lubricantsand is the direct responsibility of The apparatus described in 5.1 – 5.4 inclusive is similar in specification to the
Subcommittee D02.03 on Elemental Analysis. equipment available from Houston Atlas, Inc., 22001 North Park Dr., Kingswood,
Current edition approved May 1, 2010. Published May 2010. Originally TX 77339-3804. For further information see Drushel, H. V., “Trace Sulfur
approved in 1987. Last previous edition approved in 2004 as D4045– 04. DOI: Determination Petroleum Fractions,” Analytical Chemistry, Vol 50, 1978, p. 76.
4
10.1520/D4045-04R10. 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 to the standard’s Document Summary page on careful consideration at a meeting of the responsible technical committee, which
the ASTM website. you may attend.
Copyright © ASTM International, 100 Barr Harbo
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.