Physical Address
304 North Cardinal St.
Dorchester Center, MA 02124
D5369-93 – Standard Test Method Technical Guide
🔬 Scope and Sample Suitability
ASTM D5369–93 (Reapproved 2008) defines the standard practice for extracting nonvolatile and semivolatile organic compounds from solid matrices using Soxhlet extraction. This technique is applicable to soils, sediments, sludges, and granular solid wastes. The sample must be thoroughly dried by mixing with sodium sulfate or magnesium sulfate to ensure all surfaces are dry. Furthermore, the physical form must allow the sample to pass through a 10‑mesh sieve (approximately 2 mm openings) or have a thickness of less than 2 mm.
⚙️ Procedure and Analytical Specifications
The practice is restricted to solvents with boiling points below the boiling point of water at ambient pressure. The resulting solvent extract can be analyzed for total or specific compounds. When used in conjunction with Test Method D5368, this practice allows for the determination of the Total Solvent Extractable Content (TSEC). The standard explicitly targets extracts suitable for analysis by gas chromatography with flame ionization detection (GC/FID) or gas chromatography with mass spectrometric detection (GC/MS). Note that sample cleanup procedures may be required prior to specific compound analysis.
💡 Key Limitation: This practice is not intended for volatile organic compounds (VOCs). It is strictly for nonvolatile and semivolatile organics. Users must establish appropriate health and safety protocols (see Section 9 of the standard) prior to handling extraction solvents.
📊 Technical Specifications and Related Standards
Critical technical thresholds and the primary analysis targets defined within the standard are summarized below.
| 🟦 Parameter | 📏 Specification / Requirement |
|---|---|
| Sample Particle Size | Pass 10‑mesh sieve (~2 mm openings) or < 2 mm thickness |
| Drying Agents | Sodium sulfate or Magnesium sulfate |
| Target Analytics | Nonvolatile and Semivolatile Organic Compounds |
| Solvent Boiling Point | Below boiling point of water at ambient pressure |
| Recommended Analysis | GC/FID, GC/MS, Gravimetric (per D5368 for TSEC) |
| EPA Equivalent Method | SW‑846 Method 3540 |
The standard is closely tied to several other ASTM methods and EPA guidance documents for comprehensive waste analysis.
| 📐 Standard / Document | 🎯 Application Linkage |
|---|---|
| D5368 | Gravimetric determination of Total Solvent Extractable Content (TSEC) |
| D3694 | Preparation of sample containers and preservation of organic constituents |
| D3976 | Standard Practice for Preparation of Sediment Samples for Chemical Analysis |
| EPA SW‑846 3540 | Original EPA Soxhlet extraction method upon which the practice is based |
⚠️ Regulatory Context: The standard cites EPA SW‑846 Method 3540 as a key reference. While this ASTM practice provides a consensus framework for Soxhlet extraction, users performing compliance monitoring should verify the specific regulatory requirements of their governing jurisdiction.
❓ Frequently Asked Questions
🔍 What types of samples are suitable for extraction using ASTM D5369?
This practice is designed for solid waste samples, specifically soils, sediments, sludges, and granular solid wastes. The sample must be dry enough to mix with a drying agent (sodium or magnesium sulfate) and be physically reduced to pass through a 10‑mesh sieve (approximately 2 mm openings).
💡 Can this standard be used for volatile organic compounds (VOCs)?
No. The scope of D5369 explicitly limits its application to nonvolatile and semivolatile organic compounds. The extraction process, which involves prolonged heating, typically prevents the accurate recovery of volatile components. Alternative methods such as purge‑and‑trap or headspace analysis should be used for VOCs.
⚡ What is the relationship between D5369 and EPA Method 3540?
ASTM D5369 was developed in coordination with EPA SW‑846 Method 3540 (Soxhlet Extraction). The practice provides a standardized framework for conducting the Soxhlet extraction procedure and references Method 3540 directly. It ensures consistency and quality control when using this widely accepted extraction technique for waste characterization.
📌 What analytical techniques are recommended for the resulting extract?
The standard specifically identifies that the solvent extracts obtained are suitable for analysis by gas chromatography with flame ionization detection (GC/FID) or gas chromatography with mass spectrometric detection (GC/MS). Additionally, extracts can be used for gravimetric determination of Total Solvent Extractable Content (TSEC) when following Test Method D5368.