ASTM D129-00(2005)
(Test Method)Standard Test Method for Sulfur in Petroleum Products (General Bomb Method)
Standard Test Method for Sulfur in Petroleum Products (General Bomb Method)
ABSTRACT
This standard details the general bomb test method for determination of the amount of sulfur in lubricating oils with additives, additive concentrates, lubricating greases, and other petroleum products with low volatilities. This test method entails oxidizing samples by combustion in a bomb containing oxygen under pressure. The amount of sulfur is determined by gravimetry. Materials needed for the test include a combustion bomb, sample cup, firing wire, ignition circuit, and a cotton wicking or nylon sewing thread. All reagents, samples, and other chemicals used for the test should conform to the required concentration and purity.
SCOPE
1.1 This test method covers the determination of sulfur in petroleum products, including lubricating oils containing additives, additive concentrates, and lubricating greases that cannot be burned completely in a wick lamp. The test method is applicable to any petroleum product sufficiently low in volatility that it can be weighed accurately in an open sample boat and containing at least 0.1 % sulfur.
Note 1—This test method is not applicable to samples containing elements that give residues, other than barium sulfate, which are insoluble in dilute hydrochloric acid and would interfere in the precipitation step. These interfering elements include iron, aluminum, calcium, silicon, and lead which are sometimes present in greases, lube oil additives, or additive oils. Other acid insoluble materials that interfere are silica, molybdenum disulfide, asbestos, mica, and so forth. The test method is not applicable to used oils containing wear metals, and lead or silicates from contamination. Samples that are excluded can be analyzed by Test Method D 1552.
1.2This 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. See 3.2 for specific precautionary directions incorporated in the test method.
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British Standard 4454
Designation:D129–00 (Reapproved 2005)
Designation: 61/99
Standard Test Method for
Sulfur in Petroleum Products (General Bomb Method)
This standard is issued under the fixed designation D129; 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.
This test method has been adopted for use by government agencies to replace Method 5202 of Federal Test Method No. 791b
1. Scope* D6299 Practice for Applying Statistical Quality Assurance
and Control Charting Techniques to Evaluate Analytical
1.1 This test method covers the determination of sulfur in
Measurement System Performance
petroleum products, including lubricating oils containing addi-
E144 Practice for Safe Use of Oxygen Combustion Bombs
tives, additive concentrates, and lubricating greases that cannot
be burned completely in a wick lamp. The test method is
3. Summary of Test Method
applicable to any petroleum product sufficiently low in vola-
3.1 The sample is oxidized by combustion in a bomb
tility that it can be weighed accurately in an open sample boat
containing oxygen under pressure. The sulfur, as sulfate in the
and containing at least 0.1 % sulfur.
bomb washings, is determined gravimetrically as barium sul-
NOTE 1—This test method is not applicable to samples containing
fate.
elements that give residues, other than barium sulfate, which are insoluble
3.2 Warning—Strict adherence to all of the provisions
in dilute hydrochloric acid and would interfere in the precipitation step.
prescribed hereafter ensures against explosive rupture of the
These interfering elements include iron, aluminum, calcium, silicon, and
bomb, or a blow-out, provided the bomb is of proper design
leadwhicharesometimespresentingreases,lubeoiladditives,oradditive
and construction and in good mechanical condition. It is
oils. Other acid insoluble materials that interfere are silica, molybdenum
disulfide, asbestos, mica, and so forth.The test method is not applicable to desirable, however, that the bomb be enclosed in a shield of
usedoilscontainingwearmetals,andleadorsilicatesfromcontamination.
steel plate at least 13 mm thick, or equivalent protection be
Samples that are excluded can be analyzed by Test Method D1552.
provided against unforseeable contingencies.
1.2 This standard does not purport to address all of the
4. Apparatus and Materials
safety concerns, if any, associated with its use. It is the
3,4
responsibility of the user of this standard to establish appro- 4.1 Bomb, having a capacity of not less than 300 mL, so
constructed that it will not leak during the test and that
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. See 3.2 for specific quantitative recovery of the liquids from the bomb may be
achieved readily. The inner surface of the bomb may be made
precautionary directions incorporated in the test method.
of stainless steel or any other material that will not be affected
2. Referenced Documents
by the combustion process or products. Materials used in the
2.1 ASTM Standards: bomb assembly, such as the head gasket and lead-wire insula-
D1193 Specification for Reagent Water tion,shallberesistanttoheatandchemicalaction,andshallnot
D1552 Test Method for Sulfur in Petroleum Products undergo any reaction that will affect the sulfur content of the
(High-Temperature Method) liquid in the bomb.
4.2 Sample Cup, platinum, 24 mm in outside diameter at the
bottom, 27 mm in outside diameter at the top, 12 mm in height
outside, and weighing 10 to 11 g.
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
4.3 Firing Wire, platinum, No. 26B&S gage, 0.41 mm (16
D02.03 on Elemental Analysis.
thou), 27 SWG, or equivalent. (Warning—The switch in the
Current edition approved May 1, 2005. Published May 2005. Originally
ignition circuit shall be of a type which remains open, except
approved in 1922. Last previous edition approved in 2000 as D129 – 00.
This test method was adopted as a joint ASTM-IP standard in 1964. when held in closed position by the operator.)
In the IP, this test method is under the jurisdiction of the Standardization
Committee. DOI: 10.1520/D0129-00R05.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Criteria for judging the acceptability of new and used oxygen combustion
Standards volume information, refer to the standard’s Document Summary page on bombs are described in Practice E144.
the ASTM website. A bomb conforming to the test specifications in IP Standard IP 12 is suitable.
*ASummary of Changes section appears at the end of this standard.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D129–00 (2005)
NOTE 2—After repeated use of the bomb for sulfur determinations, a
4.4 Ignition Circuit, capable of supplying sufficient current
film may be noticed on the inner surface.This dullness can be removed by
toignitethecottonwickingornylonthreadwithoutmeltingthe
periodic polishing of the bomb.Asatisfactory method for doing this is to
wire.The current shall be drawn from a step-down transformer
rotate the bomb in a lathe at about 300 rpm and polish the inside surface
or from a suitable battery.
withemerypolishingpapersGritNo. ⁄0,orequivalentpaper, coatedwith
4.5 Cotton Wicking or Nylon Sewing Thread, white.
a light machine oil to prevent cutting, and then with a paste of grit-free
chromic oxide and water. This procedure will remove all but very deep
5. Reagents and Materials pits and put a high polish on the surface. Before the bomb is used it shall
be washed with soap and water to remove oil or paste left from the
5.1 Purity of Reagents—Reagent grade chemicals shall be
polishing operation.
used in all tests. Unless otherwise indicated, it is intended that
6.1.1 Warning—Do not use more than 1.0 g total of sample
all reagents shall conform to the specifications of the Commit-
and white oil or other low sulfur combustible material or more
tee onAnalytical Reagents of theAmerican Chemical Society,
than 0.8 g if the IP 12 bomb is used.
where such specifications are available. Other grades may be
Sulfur Content Weight of Weight of
used, provided it is first ascertained that the reagent is of
percent Sample, g White Oil, g
sufficiently high purity to permit its use without lessening the
accuracy of the determination.
5 or under 0.6 to 0.8 0.0
Over 5 0.3 to 0.4 0.3 to 0.4
5.2 Purity of Water—Unless otherwise indicated, references
to water shall mean water as defined by Type II or III of
NOTE 3—Useofsampleweightscontainingover20mgofchlorinemay
Specification D1193. cause corrosion of the bomb. To avoid this, it is recommended that for
samples containing over 2 % chlorine, the sample weight be based on the
5.3 Barium Chloride Solution (85 g/litre)—Dissolve 100 g
chlorine content as given in the following table:
of barium chloride dihydrate (BaCl ·2H O) in distilled water
2 2
Chlorine Content Weight of Weight of
and dilute to 1 litre.
percent Sample, g White Oil, g
5.4 Bromine Water (saturated).
5.5 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro- 2to5 0.4 0.4
Over 5 to 10 0.2 0.6
chloric acid (HCl).
Over 10 to 20 0.1 0.7
5.6 Oxygen, free of combustible material and sulfur com-
Over 20 to 50 0.05 0.7
pounds, available at a pressure of 41 kgf/cm (40 atm).
NOTE 4—If the sample is not readily miscible with white oil, some
5.7 SodiumCarbonateSolution(50g/litre)—Dissolve135g
other low sulfur combustible diluent may be substituted. However, the
of sodium carbonate decahydrate (Na CO ·10H O) or its
2 3 2
combined weight of sample and nonvolatile diluent shall not exceed 1.0 g
equivalent weight in distilled water and dilute to 1 litre.
or more than 0.8 g if the IP 12 bomb is used.
5.8 White Oil, USP, or Liquid Paraffın,BP, or equivalent.
6.2 Addition of Oxygen—Place the sample cup in position
5.9 Quality Control (QC) Samples, preferably are portions
andarrangethecottonwispornylonthreadsothattheenddips
of one or more liquid petroleum materials that are stable and
into the sample. Assemble the bomb and tighten the cover
representative of the samples of interest. These QC samples
securely. (Warning—Do not add oxygen or ignite the sample
can be used to check the validity of the testing process as
if the bomb has been jarred, dropped, or tilted.)Admit oxygen
described in Section 10.
slowly (to avoid blowing the oil from the cup) until a pressure
is reached as indicated in the following table:
6. Procedure
Capacity of Minimum Gage Maximum Gage
A 2 A 2
6.1 Preparation of Bomb and Sample—Cutapieceoffiring Bomb, ml Pressure, kgf/cm (atm) Pressure, kgf/cm (atm)
wire 100 mm in length. Coil the middle section (about 20 mm)
300 to 350 39 (38) 41 (40)
and attach the free ends to the terminals. Arrange the coil so
350 to 400 36 (35) 38 (37)
that it will be above and to one side of the sample cup. Insert 400 to 450 31 (30) 33 (32)
450 to 500 28 (27) 30 (29)
between two loops of the coil a wisp of cotton or nylon thread
A
The minimum pressures are specified to provide sufficient oxygen for com-
of such length that one end will extend into the sample cup.
plete combustion and the maximum pressures represent a safety requirement.
Placeabout5mLofNa CO solutioninthebomb(Note2)and
2 3
6.3 Combustion—Immerse the bomb in a cold distilled-
rotate the bomb in such a manner that the interior surface is
water bath. Connect the terminals to the open electrical circuit.
moistened by the solution. Introduce into the sample cup the
Close the circuit to ignite the sample. (Warning—Do not go
quantities of sample and white oil (Note 3 and Note 4)
nearthebombuntilatleast20safterfiring.)Removethebomb
specified in the following table, weighing the sample to the
from the bath after immersion for at least 10 min. Release the
nearest 0.2 mg (when white oil is used, stir the mixture with a
short length of quartz rod and allow the rod to remain in the
sample cup during the combustion). 6
The sole source of supply of the apparatus known to the committee at this time
is Emery Polishing Paper Grit No. ⁄0
...
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