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ASTM D874 - Sulfated Ash from Lubricating Oils and Additives

Significance and Use

5.1 The sulfated ash can be used to indicate the concentration of known metal-containing additives in new oils. When phosphorus is absent, barium, calcium, magnesium, sodium and potassium are converted to their sulfates and tin (stannic) and zinc to their oxides (Note 4). Sulfur and chlorine do not interfere, but when phosphorus is present with metals, it remains partially or wholly in the sulfated ash as metal phosphates.

NOTE 4: Since zinc sulfate slowly decomposes to its oxide at the ignition temperature specified in the test method, samples containing zinc can give variable results unless the zinc sulfate is completely converted to the oxide.

5.2 Because of above inter-element interferences, experimentally obtained sulfated ash values may differ from sulfated ash values calculated from elemental analysis. The formation of such non-sulfated species is dependent on the temperature of ashing, time ashed, and the composition of metal compounds present in oils. Hence, sulfated ash requirement generally should not be used in product specifications without a clear understanding between a buyer and a seller of the unreliability of an ash value as an indicator of the total metallic compound content.

1. Scope

1.1 This test method covers the determination of the sulfated ash from unused lubricating oils containing additives and from additive concentrates used in compounding. These additives usually contain one or more of the following metals: barium, calcium, magnesium, zinc, potassium, sodium, and tin. The elements sulfur, phosphorus, and chlorine can also be present in combined form.

1.2 Application of this test method to sulfated ash levels below 0.02 % by mass  is restricted to oils containing ashless additives. The lower limit of the test method is 0.005 % by mass sulfated ash.

NOTE 1: This test method is not intended for the analysis of used engine oils or oils containing lead. Neither is it recommended for the analysis of nonadditive lubricating oils, for which Test Method D482 can be used.

NOTE 2: There is evidence that magnesium does not react the same as other alkali metals in this test. If magnesium additives are present, the data is interpreted with caution.

NOTE 3: There is evidence that samples containing molybdenum can give low results because molybdenum compounds are not fully recovered at the temperature of ashing.

1.3 Fatty acid methyl ester (FAME) conforming to EN 14213 and EN 14214, when tested using this test method, were shown to meet its precision.

1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.

Extracted, with permission, from ASTM D874-13a - Sulfated Ash from Lubricating Oils and Additives, copyright ASTM International, 100 Barr Harbor Drive, West Conshohocken, PA 19428. A copy of the complete standard may be purchased from ASTM International, astm.org