An American National Standard British Standard 4454
Standard Test Method for
Sulfur in Petroleum Products (General Bomb Method)1
This standard is issued under the ﬁxed designation D 129; 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 inparentheses indicates the year of last reapproval. A superscript epsilon (e) 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 1.1 This test method covers the determination of sulfur in petroleum products, including lubricating oils containingadditives, 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 bariumsulfate, 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, etc. The test method is not applicable to used oilscontaining wear metals, and lead or silicates from contamination. Samples that are excluded can be analyzed by Test Method D 1552.
Techniques to Evaluate Analytical Measurement System Performance4 E 144 Practice for Safe Use of Oxygen Combustion Bombs5 3. Summary of Test Method 3.1 The sample is oxidized by combustion in a bomb containing oxygen under pressure. The sulfur, as sulfate in thebomb washings, is determined gravimetrically as barium sulfate. 3.2 Warning— Strict adherence to all of the provisions prescribed hereafter ensures against explosive rupture of the bomb, or a blow-out, provided the bomb is of proper design and construction and in good mechanical condition. It is desirable, however, that the bomb be enclosed in a shield of steel plate at least 13 mm thick, orequivalent protection be provided against unforseeable contingencies. 4. Apparatus and Materials 4.1 Bomb,6,7 having a capacity of not less than 300 mL, so constructed that it will not leak during the test and that quantitative recovery of the liquids from the bomb may be achieved readily. The inner surface of the bomb may be made of stainless steel or any other material that will not be affected by thecombustion process or products. Materials used in the bomb assembly, such as the head gasket and lead-wire insulation, shall be resistant to heat and chemical action, and shall not undergo any reaction that will affect the sulfur content of the 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, andweighing 10 to 11 g. 4.3 Firing Wire, platinum, No. 26 B & S gage, 0.41 mm (16 thou), 27 SWG, or equivalent. (Warning—The switch in the ignition circuit shall be of a type which remains open, except
1.2 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 safetyand health practices and determine the applicability of regulatory limitations prior to use. See 3.2 for speciﬁc precautionary directions incorporated in the test method. 2. Referenced Documents 2.1 ASTM Standards: D 1193 Speciﬁcation for Reagent Water2 D 1552 Test Method for Sulfur in Petroleum Products (High-Temperature Method)3 D 6299 Practice for Applying Statistical Quality Assurance...