D5353-95 – Standard Test Method Technical Guide

📌 Scope and Referenced Documents

ASTM D5353-95 (Reapproved 2019) is a standard test method for the determination of total desulfated fatty matter in sulfated oils. The method is derived from Sections 29 through 32 of Test Methods D500. It achieves this by decomposing the sample with diluted mineral acids and extracting the decomposed fat with a solvent. The standard explicitly states that it is not applicable to samples that do not completely decompose upon boiling with mineral acids.

The test method is under the jurisdiction of ASTM Committee D31 on Leather and is the direct responsibility of Subcommittee D31.08 on Fats and Oils. Referenced documents include D500, D5350, and D5351.

⚙️ Reagents and Step-by-Step Procedure

The procedure involves the quantitative decomposition of the sulfated oil, followed by liquid-liquid extraction to isolate the fatty matter.

Reagents

🧪 Reagent📐 Specification
Ethyl EtherAnhydrous, for extraction of fatty matter.
Sulfuric Acid (1+19)Carefully mix 1 volume of concentrated H₂SO₄ (sp gr 1.84) into 19 volumes of water.

Procedure

The procedure begins with the titrated solution obtained from the determination of organically combined sulfuric anhydride in accordance with Test Method D5350 or D5351.

  1. Extraction: Transfer the titrated solution (6.1.2) into a 250 mL separatory funnel and shake with 50 mL of ethyl ether. Draw off the water layer into a second separatory funnel and extract it twice with 25 mL portions of ether.
  2. Washing: Wash the combined ether layers with

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