Overview
ISO 11916-1:2013 - "Soil quality - Determination of selected explosives and related compounds - Part 1: Method using high‑performance liquid chromatography (HPLC) with ultraviolet detection" - specifies a validated laboratory procedure for the trace analysis of explosive and related nitrocompounds in soils. The method uses reversed‑phase HPLC with a diode array/UV detector (DAD/UV) to quantify compounds such as TNT, RDX, HMX, DNT isomers, nitrobenzene and other nitroaromatics. Under the specified conditions, the method can determine concentrations in the approximate range 0.1 mg/kg to 1 mg/kg (dry matter), depending on the analyte.
Key topics and technical requirements
- Target analytes: Selected explosives and related nitrocompounds (see Table 1 for specific compounds). Note: PETN, 1,3,5‑TNB and tetryl showed problematic interlaboratory results and may be difficult to analyze.
- Extraction techniques: Ultrasonic extraction (USE), mechanical shaking (MSE), Soxhlet (SOX) or pressurized liquid extraction (PLE) using acetonitrile or methanol.
- Chromatography: Reversed‑phase HPLC with DAD/UV (wavelength range ~200–400 nm), pump capable of ≥40 MPa, injection loop ~100 µL.
- Reagents & standards: HPLC‑grade acetonitrile, methanol, water; single‑substance and multi‑component stock solutions; method‑checking standard (e.g., 2,5‑DNT). Calibration requires a minimum of five concentration levels.
- Sample handling: Remove coarse debris, sieve to 2 mm, determine water/dry matter content, store at (4 ± 2) °C if analysed within 1 week or at −20 °C for longer storage. Special handling for volatile nitroaromatics (on‑site methanol preservation or dedicated sample withdrawal).
- Interferences & precautions: Demonstrate blank‑free solvents and labware; tetryl may decompose in methanol/water and can interfere with TNT quantification; acetonitrile extraction of samples containing 2,4,6‑trinitrobenzoic acid can overestimate 1,3,5‑TNB due to decarboxylation.
- Quality assurance: Method blanks, recovery checks, precision data (annexed), and reporting requirements are specified.
Applications and who uses it
- Environmental laboratories performing soil contamination assessments and remediation monitoring.
- Regulatory agencies and consultants assessing sites impacted by military activity, munitions disposal, or industrial nitroaromatic contamination.
- Research institutions studying fate, transport and degradation products of explosives in soils.
- Useful for risk assessment, site characterization, compliance testing and remediation verification where reliable HPLC‑UV trace analysis is required.
Related standards
- ISO 11916‑2 - complementary GC methods (ECD or MS) for explosives in soil.
- ISO 22478 - HPLC‑UV method for explosives in water (mobile phase/system guidance referenced).
- ISO standards for sample sieving and dry matter determination used in the procedure (e.g., ISO 565, ISO 11465).
Keywords: ISO 11916-1:2013, soil quality, explosives in soil, HPLC‑UV, nitrocompounds, TNT, RDX, environmental testing, trace analysis.
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