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D5354-95 – Standard Test Method Technical Guide
🔬 Scope and Significance
ASTM D5354-95 (Reapproved 2020) provides a standard test method for determining the total active ingredients in sulfonated and sulfated oils. The procedure extracts undecomposed sulfonated/sulfated fat and other fatty matter over an acidified concentrated salt solution, explicitly excluding free alkali and alkali bound as soap. Derived from Test Methods D500, this method relies on a gravimetric approach to quantify the fatty matter as it exists in the original oil sample. This 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.
📏 Standard Compliance: The values stated in SI units are to be regarded as standard. Users are responsible for establishing appropriate safety, health, and environmental practices prior to use.
🧪 Reagents, Procedure, and Parameters
The accuracy of this test method depends on specific reagents and strict adherence to the drying procedure to ensure proper isolation and stabilization of the active ingredients.
| 🟦 Reagent | 📏 Specification | 📐 Key Notes |
|---|---|---|
| Ethyl Ether | Technical grade | Used to dissolve the sample |
| Methyl Orange Indicator Solution | 1 g/L (0.1 g in 100 mL H₂O) | Standard indicator for pH titration |
| Sodium Chloride (NaCl) | Solid | Prepared as saturated brine for washing |
| Sodium Sulfate (Na₂SO₄) | Anhydrous | Used as a drying agent |
| Alcoholic KOH Solution | 0.5 N Standardized | 1 mL = 28.05 mg KOH; used for stabilization |
The procedure begins by isolating the fatty matter from the oil sample. Proceed as described in Test Method B for the determination of organically combined sulfuric anhydride in the absence of ammonia, retaining the separated active ingredients in a 150-mL beaker. The filtrate is evaporated to a total volume of about 20 mL. Exactly 2 mL of the 0.5 N alcoholic KOH solution is added, the contents are mixed by swirling, and the sample is evaporated until practically free from ether.
⚡ Highly Sulfonated Oils: With highly sulfonated or sulfated oil, it may be necessary to add 5 to 10 mL of the alcoholic KOH solution to stabilize the residue (see Note 2).
The residue is dried in an oven at 108 to 112°C for 1.5 hours. It is then cooled in a desiccator and weighed. The process is repeated with 30-minute heating periods until a constant weight is obtained.
📊 Calculation and Reporting
The final calculation corrects for the alkali added during the procedure. The standard formula (Section 6.1) subtracts the weight of the KOH added from the dried residue to derive the true total active ingredients. For sulfated oils alone, the result may also be calculated as the sum of the desulfated fatty matter and the neutralized organically combined sulfuric anhydride.
| ⚡ Parameter | 🎯 Required Value / Instruction |
|---|---|
| KOH Volume (Standard Oil) | 2 mL of 0.5 N alcoholic solution |
| KOH Volume (Highly Sulfonated) | 5–10 mL of 0.5 N alcoholic solution |
| Drying Temperature | 108 – 112 °C |
| Initial Drying Duration | © 2026 TNLab — This article is a technical interpretation for reference only. The original standard as published by ASTM International takes precedence. 📥 Standard Documents Download |