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These test methods cover the chemical analysis of sulfonated and sulfated oils. Water by distillation with volatile solvent and moisture and volatile matter by hot-plate shall be tested to meet the requirements prescribed. Titration test, extraction-titration test, and ash-gravimetric test shall be performed to meet the requirements specified. Total desulfated fatty matter, total active ingredients, unsaponifiable non-volatile matter, inorganic salts, total alkalinity, and total ammonia shall be tested to meet the requirements prescribed. In the absence of ammonium or triethanolamine soaps test method, brine test method, and in the presence of ammonium or triethanolamine soaps test method shall be performed to meet the requirements prescribed. Water-immiscible organic solvents volatile with steam shall be tested to meet the requirements prescribed.

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1.1 These test methods cover the chemical analysis of sulfonated and sulfated oils. The analytical procedures appear in the following order:

Section Moisture: Test Method A. Water by Distillation with Volatile Solvent4-9 Test Method B. Moisture and Volatile Matter by Hot-Plate Method10-14 Organically Combined Sulfuric Anhydride: Test Method A. Titration Test15-19 Test Method B. Extraction-Titration Test20-24 Test Method C. Ash-Gravimetric Test (in the Presence of True
Sulfonates)25-28 Total Desulfated Fatty Matter29-32 Total Active Ingredients33-36 Unsaponifiable Nonvolatile Matter37-41 Inorganic Salts42-46 Total Alkalinity47-49 Total Ammonia50-52 Acidity as Free Fatty Acids or Acid Number: Test Method A. In the Absence of Ammonium or Triethanolamine Soaps53-56 Test Method B. In the Presence of Dark Colored Oils but in the
Absence of Ammonium or Triethanolamine Soaps (Brine Test)57-60 Test Method C. In the Presence of Ammonium or Triethanolamine Soaps61-63 Water-Immiscible Organic Solvents Volatile with Steam64-70

1.2 The values stated in inch-pound units are to be regarded as the standard. The metric equivalents of inch-pound units may be approximate.

1.3 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. Material Safety Data Sheets are available for reagents and materials. Review them for hazards prior to usage.

4.1 This test method covers the determination of water existing in a sample of sulfonated or sulfated oil, or both, by distilling the sample with a volatile solvent. The method is applicable only to sulfonated and sulfated oils that do not contain the following: mineral acids, free sulfonic acids, or free sulfuric acid esters; or alkali hydroxides, carbonates or acetates; or alcohol, glycerin, diethylene glycol, acetone, or other water-miscible volatile compounds.

10.1 This test method covers the determination of the percentage of water and other compounds volatile at about 100°C existing in a sample of sulfonated or sulfated oil, or both, by rapid evaporation. The test method is applicable only to sulfonated and sulfated oils that do not contain the following: mineral acids, free sulfonic acids or free sulfuric acid esters, ammonia, acetic acid or similar volatile acids, alkali hydroxides, carbonates, acetates or similar salts that may react with oleic acid at elevated temperatures liberating volatile acids, or glycerin, diethylene glycol, xylene, or other compounds of similar volatility.

15.1 This test method covers the determination of the organically combined sulfuric anhydride existing in a sample of sulfated oil by boiling the sample with sulfuric acid and determining the acidity of the reaction mixture. This method is applicable only to oils that split off their combined SO₃ upon boiling with mineral acids and that do not contain compounds that cannot be accurately titrated in water solution with methyl orange as the indicator.

20.1 This test method covers the determination of the organically combined sulfuric anhydride existing in a sample of sulfated oil by extracting the undecomposed sulfated fat and other fatty matter over an acidulated, concentrated salt solution, boiling the residue with sulfuric acid after evaporating the solvent, and titrating the products of reaction. This method is applicable only to sulfated oils that split off their combined SO₃ upon boiling with mineral acids, including samples containing sodium acetate or other compounds that cannot be accurately titrated in water solution with methyl orange as the indicator.

25.1 This test method covers the determination of the organically combined sulfuric anhydride existing in a sample of sulfonated or sulfated oil, or both, by extracting the undecomposed sulfonated or sulfated fat and other fatty matter over an acidulated, concentrated salt solution, and ashing the purified extract. This test method is applicable to all types of sulfonated and sulfated oils, including true sulfonic acid oils and those containing sodium acetate or similar partially titratable compounds.

29.1 This test method covers the determination of the total desulfated fatty matter in a sample of sulfated oil by decomposition with diluted mineral acids and extraction of the decomposed fat. This test method is not applicable to samples that are not completely decomposed upon boiling with mineral acids.

33.1 This test method covers the determination of the total active ingredients in a sample of sulfonated or sulfated oil, or both, as it exists in the original sample by extracting the undecomposed sulfonated or sulfated fat and other fatty matter over an acidified concentrated salt solution. Free alkali or alkali bound as soap is not included.

Note 5—In the case of sulfated oils only, this determination may also be estimated by calculation (see 36.3), as it is equivalent to the sum of the desulfated fatty matter and neutralized organically combined sulfuric anhydride.

37.1 This test method covers the determination of the unsaponifiable, nonvolatile (above 80°C) matter existing in a sample of sulfated oil by saponifying the desulfated fatty matter and extracting the unsaponifiable matter from the soap solution with ethyl ether.

42.1 This test method covers the determination in a sample of sulfonated or sulfated oil, or both, the inorganic sulfates, chlorides, and all other salts that are insoluble in a mixture of oleic acid and chloroform.

47.1 This test method covers the determination of the total alkalinity existing in a sample of sulfonated or sulfated oil, or both, by titrating a water solution of the sample with mineral acid in the presence of methyl orange as the indicator. This test method covers the determination of the total alkalinity of the fixed alkali, ammonia and triethanolamine bound as soap, free alkali, and the alkalinity of titratable alkaline salts, but not that of nontitratable alkaline salts.

50.1 This test method covers the determination of the total ammonia in a sample of sulfonated or sulfated oil, or both, by boiling a water solution of the sample with excess alkali and determining by titration the loss in alkali after the boiling.

53.1 This method of analysis covers the determination of the acidity as free fatty acids existing in a sample of sulfonated or sulfated oil or both by titrating the sample dissolved in a solvent. It is not applicable in the presence of ammonium or triethanolamine soaps or salts, or other compounds that do not react neutral to phenolphthalein when dissolved in alcohol.

57.1 This test method covers the determination of the acidity as free fatty acids existing in a sample of sulfonated or sulfated oil or both by titrating a water solution of the sample with phenolphthalein as the indicator. It is not applicable in the presence of ammonia or triethanolamine soaps or acid salts.

61.1 This test method covers the determination of the acidity as free fatty acids in the presence of ammonium or triethanolamine soaps, or both, existing in a sample of sulfonated or sulfated oils, or both, by calculation from the total alkalinity and the free-and-alkali-combined fatty acids.

64.1 This test method covers the determination of water-immiscible organic solvents that are volatile with steam existing in a sample of sulfonated or sulfated oil, or both. Alcohol or other volatile compounds that are mutually soluble in water and solvents interfere in this test method.