During its Test Method Revision Section Meeting held in Orlando, FL on December 06, 2022; D02.03 (Elemental Analysis) test methods that were thought to be obsolete or not being used by the petroleum community were considered. D129 was identified as possibly falling into one or both categories. D129 is a jointed test method with the Energy Institute’s test method IP 61. Energy Institute members/leadership responsible for IP 61 were contacted and agreement was found. Accordingly, this standard was balloted for withdrawal with no replacement.
D129 (first approved in 1922) is a test method with a limited scope for total sulfur in the 0.09 % to 5.5 % by mass range. The summary of the test method informs that the sample is oxidized by combustion in a high pressure decomposition device containing oxygen under pressure. The sulfur, as sulfate in the high-pressure decomposition device washings, is determined gravimetrically as barium sulfate. A suitable warning is also provided; “(Warning—Strict adherence to all of the provisions prescribed hereafter ensures against explosive rupture of the high-pressure decomposition device, or a blow-out, provided the high pressure decomposition device is of proper design and construction and in good mechanical condition. It is desirable, however, that the high-pressure decomposition device be enclosed in a shield of steel plate at least 13 mm thick, or equivalent protection be provided against unforeseeable contingencies.)” No precision and bias studies have been conducted since the 1960s and no volunteers have surfaced that are willing to revise or improve test method performance. The test method’s limited scope, relatively high safety risk and poor relative performance as compared to other D02.03 standards that measure total sulfur in petroleum and related products, may explain its perceived obscurity and obsolescence.
Formerly under the jurisdiction of Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants, this test method was withdrawn in October 2023.
РефератThis 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.
Область применения1.1 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 D1552.
1.2 This test method is applicable to samples with the sulfur in the range 0.09 % to 5.5 % by mass.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.