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法医学の研究機関は、テロ攻撃や戦闘剤の犯罪行為を追跡するために、使用された爆発物とその残留物の微量検出分析を行います。爆発物の主成分は、酸化剤と燃料であり、これには酸化物（塩素酸塩、過塩素酸塩など）や硝酸塩、硫黄、リンを含む化合物、金属、糖類、炭化水素などが含まれます[1]。典型的な無機後爆発残渣には、チオシアン酸塩やチオ硫酸塩が含まれます。特に重要なのは、犯罪捜査部門や政府の安全保障機関が「化学的な指紋」を取得することです。公衆衛生機関や環境保護機関は、これらの化合物が基盤となる土壌を汚染し、地下水に浸透する可能性があるため、これらの化合物を分析します。サプレッサを伴った伝導度検出器を搭載したイオンクロマトグラフィ（IC）では、一般的な無機アニオンに加えて、塩酸塩、チオ硫酸塩、チオシアン酸塩、過塩素酸塩などの陰イオン汚染物質を広範囲の濃度範囲で感度良く、堅牢に定量することができます。

Compact, user-friendly Metrohm IC instrumentation to quantify various anions in explosives and explosion residues.
Figure 1. Compact, user-friendly Metrohm IC instrumentation to quantify various anions in explosives and explosion residues.

Artificial samples were dissolved in 10% methanol and automatically filtered using Inline Ultrafiltration. The Metrohm intelligent Partial Loop Injection Technique (MiPT) allows the injection of a precise variable volume depending on the sample load, and an automatic calibration.

The anions are separated on the analytical column Metrosep A Supp 4 - 250/4.0 using a sodium carbonate / sodium hydrogen carbonate eluent and a flow gradient (Figure 1).

Sequential suppression, including chemical and CO2-suppression, reduces the background conductivity to around 1 μS/cm and vastly improves the signal-to-noise ratio. All anions are determined with a conductivity detector and quantified with the MagIC Net software.

Figure 2. Suppressed conductivity signal of inorganic anions (1 mg/L), separated on a Metrosep A Supp 4 - 250/4.0 column (eluent: 1.8 mmol/L sodium carbonate, 1.7 mmol/L sodium hydrogen carbonate, flow gradient 0.7–1.5 mL/min, column temperature 30 °C, sample volume 10 μL).

The developed IC method offers a straightforward, robust, and fast analysis of anionic additives and residuals related to explosives. Figure 2 displays the chromatogram of a 1 mg/L standard solution. The method covers the specifications shown in Table 1.

Table 1. Method specifications
Parameter Specification
LOQ ≤ 1mg/L for each anion, RSD ≤ 25%
Calibration Anions = 1–100 mg/L
Perchlorate = 1–50 mg/L
Resolution ≥ 2 for each separation
Blank < 0.1 mg/L
Run time 32 min

A flow gradient accelerates late-eluting components, which shortens analysis time to 32 minutes and improves peak shapes. The added methanol in the sample matrix did not interfere with the analysis in any way. For all components, the limit of quantification was below 1 mg/L and the resolution was above 2 for the full calibration range.

Using the Metrosep A Supp 4 column at ambient temperature enables the analysis with a compact IC system. For a comprehensive explosive characterization including the above specified anions as well as for cations, a two channel professional system provides a profitable solution.

Advanced studies of explosive residues are performed with IC-MS (ion chromatography coupled to mass spectrometry) to additionally confirm the analyte’s identification with a mass detector [2].

  1. Dicinoski et al. (2006), Analytical Letters, 39(4), 639–657.
  2. Barron et al. (2014), Analytica Chimica Acta 806 (2014) 27–54.
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Internal reference: AW IC FR6-0100-062017