ASTM D5705-95(2000)e1
(Test Method)Standard Test Method for Measurement of Hydrogen Sulfide in the Vapor Phase Above Residual Fuel Oils
Standard Test Method for Measurement of Hydrogen Sulfide in the Vapor Phase Above Residual Fuel Oils
SCOPE
1.1 This test method covers the field determination of hydrogen sulfide (H S) in the vapor phase (equilibrium headspace) of a residual fuel oil sample.
1.2 The test method is applicable to liquids with a viscosity range of 5.5 mm /s at 40°C to 50 mm /s at 100°C. The test method is applicable to fuels conforming to Specification D396 Grade Nos. 4, 5 (Heavy), and 6.
1.3 The applicable range is from 5 to 4000 parts per million by volume (ppm v/v) (micro mole/mole).
1.4 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.5 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.
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An American National Standard
e1
Designation: D 5705 – 95 (Reapproved 2000)
Standard Test Method for
Measurement of Hydrogen Sulfide in the Vapor Phase
Above Residual Fuel Oils
This standard is issued under the fixed designation D 5705; 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.
e NOTE—Warning notes were placed in the text in April 2000.
1. Scope 3.1.2.1 Discussion—Under the conditions of this test (1:1
liquid/vapor ratio, temperature, and agitation) the H Sinthe
1.1 This test method covers the field determination of 2
vapor phase (sample’s headspace) will be in equilibrium with
hydrogen sulfide (H S) in the vapor phase (equilibrium head-
the H S in the liquid phase.
space) of a residual fuel oil sample. 2
1.2 The test method is applicable to liquids with a viscosity
4. Summary of Test Method
2 2
range of 5.5 mm /s at 40°C to 50 mm /s at 100°C. The test
4.1 A 1-L H S-inert test container (glass test bottle) is filled
method is applicable to fuels conforming to Specification
to 50 volume % with fuel oil from a filled H S-inert container
D 396 Grade Nos. 4, 5 (Heavy), and 6.
(glass sample bottle) just prior to testing. In the test container,
1.3 The applicable range is from 5 to 4000 parts per million
the vapor space above the fuel oil sample is purged with
by volume (ppm v/v) (micro mole/mole).
nitrogen to displace air. The test container with sample is
1.4 The values stated in SI units are to be regarded as the
heated in an oven to 60°C, and agitated on an orbital shaker at
standard. The values given in parentheses are for information
220 rpm for 3 min.
only.
4.2 A length-of-stain detector tube and hand-operated pump
1.5 This standard does not purport to address all of the
are used to measure the H S concentration in the vapor phase
safety concerns, if any, associated with its use. It is the
of the test container. The length-of-stain detector tube should
responsibility of the user of this standard to establish appro-
be close to but not in contact with the liquid surface.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
5. Significance and Use
2. Referenced Documents 5.1 Excessive levels of hydrogen sulfide in the vapor phase
above residual fuel oils in storage tanks may result in a health
2.1 ASTM Standards:
2 hazard, OSHA limits violation, and public complaints about
D 396 Specification for Fuel Oils
odors. Control measures to maintain safe levels of H Sinthe
D 4057 Standard Practice for Manual Sampling of Petro-
3 tank atmosphere for those working in the vicinity require a
leum and Petroleum Products
consistent method for the assessment of potentially hazardous
3. Terminology levels of H S in fuel oils (Warning—H S is a highly toxic
2 2
substance. Use extreme care in the sampling and handling of
3.1 Definitions:
samples that are suspected of containing high levels of H S.).
3.1.1 equilibrium headspace, n—the vapor space above the
5.2 This test method has been developed to provide refin-
liquid in which all vapor components are in equilibrium with
eries, fuel terminals, and independent testing laboratories,
the liquid components.
which do not have access to analytical instruments such as a
3.1.2 residual fuel oil, n—a fuel oil comprising a blend of
gas chromatograph, with a simple and consistent field test
viscous long, short, or cracked residue from a petroleum
method for the rapid determination of H S in the vapor phase
refining process and lighter distillates blended to a fuel oil
of residual fuel oils.
viscosity specification.
5.3 This test method does not necessarily simulate the vapor
phase H S concentration of a fuel storage tank. It does,
This test method is under the jurisdiction of ASTM Committee D02 on however, provide a level of consistency so that the test result is
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
only a function of the residual fuel oil sample and not the test
D02.E0.01 on Burner Fuels.
method, operator, or location. No general correlation can be
Current edition approved May 15, 1995. Published July 1995.
established between this field test and actual vapor phase
Annual Book of ASTM Standards, Vol 05.01.
Annual Book of ASTM Standards, Vol 05.02.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 5705
concentrations of H S in residual fuel oil storage or transports.
However, a facility that produces fuel oil from the same crude
source under essentially constant conditions might be able to
develop a correlation for its individual case.
6. Interferences
6.1 Typically, sulfur dioxide and mercaptans may cause
positive interferences. In some cases, nitrogen dioxide can
cause a negative interference. Most detector tubes will have a
precleanse layer designed to remove certain interferences up to
some maximum interferant level. Consult the manufacturer’s
instructions for specific interference information.
7. Apparatus
7.1 Shaker, a bench-top orbital shaker and platform
equipped with a four-prong clamp to hold 1-L Boston round-
bottom glass bottles and capable of operation at 220 rpm.
7.2 Timer, capable of measuring from1sto30min at
second intervals.
7.3 Stopper with Thermometer, a No. 2 cork stopper with a
dial thermometer having a range of − 18 to 82°C and a 200-
mm stem. The thermometer is inserted through the stopper
such that the stem will extend at least 25 mm into the fuel but
be no closer than 25 mm from the bottom of a test bottle (Fig.
1(a)).
7.4 Oven or Water Bath, capable of heating the fuel oil
samples to 60 6 1°C.
7.5 Detector Tube Pump, a hand-operated piston or bellows-
3 3
type (Fig. 1(b)) pump with a capacity of 100 cm 6 5cm per
stroke. It must be specifically designed for use with detector
tubes (Warning—A detector tube and pump together form a
unit and must be used as such. Each manufacturer calibrates
FIG. 1 Measurement of H S in the Vapor Phase of Residual Fuel
detector tubes to match the flow characteristics of its specific
Oil
pump. Crossing brands of pumps and tubes is not permitted, as
considerable loss of system accuracy is likely to occur.).
containing hydrogen sulfide. Any substances known to inter-
fere must be listed in the instructions accompanying the tubes.
8. Reagents and Materials
A calibration scale should be marked directly on the tube, or
8.1 Containers—Both sample and test containers are com-
other markings that provide for easy interpretation (reading) of
posed of H S-inert material such as 1-L size (clear Boston
hydrogen sulfide content from a separate calibration scale
round-bottom) glass bottles with screw caps. The bottles are
should be supplied with the tubes. The calibration scale shall
clean and dry. Mark test containers at the 50 % volume level by
correlate H S concentration to the length of the color stain.
using a ruler (Warning—Hydrogen sulfide reacts with metal
Annex A1 provides additional information. Shelf life of the
surfaces and is easily oxidized, which depletes its concentra-
detector tubes must be a minimum of two years from the date
tion and gives false low test results. Containers such as
of manufacture, when stored according to the manufacturer’s
epoxy-lacquered cans are suitable for sample collection. Alter-
recommendations.
native containers must give equivalent results to those obtained
by using glass.).
9. Sampling
8.2 Length-of-Stain Detector Tube and Calibration Scale,a
9.1 The sampling of residual fuel oils is done according to
sealed glass tube with breakoff tips sized to fit the tube holder
Practice D 4057 for the sampling of storage tanks, ships, or
of the detector tube pump. The reagent layer inside the tube,
barges. Composite sampling or running samples can be taken;
typically a silica gel substrate coated with the active chemicals,
spot samples should be taken from the midpoint or below
must be specific for hydrogen sulfide and must produce a
midpoint of the fuel oil in a storage tank by first sufficiently
distinct color change when exposed to a sample of gas
purging sample transfer lines and then taking single samples
where each sample comprises one and only one test
(Warning—Samples taken for this test method shall be dedi-
Baxter Scientific Product Models 3518 and 30100, or equivalent, are suitable
cated to a single H S determination and not used for any other
for this test.
purpose, as any additional handling can lead to loss of H S and
Direct Reading Colorimetric Indicator Tubes Manual, First Edition, American 2
Industrial Hygiene Association, Akron, OH 44311, 1976. thus low results.).
D 5705
NOTE 1—Liquid samples taken well into the fuel oil have had less H S
only contacting the sample’s vapor phase. Do not allow the
lost by degassing as compared with a fuel oil’s surface. Samples taken
detector tube to contact the liquid, see Fig. 1(b). Use one full
from well within the fuel oil storage provide material that represents the
compression stroke.
greatest potential for H S exposure during fuel oil movements. Hydrogen
10.9 Remove the detector tube after complete decompres-
sulfide is lo
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