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Characterization, Quantification and Compound-specific Isotopic Analysis of Pyrogenic Carbon Using Benzene Polycarboxylic Acids BPCA

Characterization, Quantification and Compound-specific Isotopic Analysis of Pyrogenic Carbon Using Benzene Polycarboxylic Acids BPCA

Published on: May 16, 2016

Compound-specific carbon isotope analysis for mechanistic characterization of debromination of decabrominated

Xifen Zhu^1,2, Yin Zhong¹, Heli Wang^1,2

¹Guangdong Provincial Key Laboratory of Environmental Protection and Resources Utilization, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, State Key Laboratory of Organic Geochemistry, Guangzhou, 510640, China.

Rapid Communications in Mass Spectrometry : RCM

|February 18, 2020

Abstract

Rationale:

Decabrominated diphenyl ether (BDE-209) is a notorious persistent organic pollutant widely found in the environment. Developing a compound-specific isotope analysis (CSIA) method is much needed in order to trace its transport and degradation processes and to evaluate the effectiveness of the remediation of BDE-209 in the environment. However, the conventional CSIA method, i.e. gas chromatography (GC) combustion isotope ratio mass spectrometry, is not appropriate for BDE-209 because of its high thermal instability and incomplete combustion.

Methods:

We developed a high-performance liquid chromatography (HPLC) method for the separation and purification of BDE-209 that prevents its thermal reactivity as occurred in prior GC-based methods. The δ¹³ C value of the purified BDE-209 was determined using offline elemental analyzer isotope ratio mass spectrometry (EA/IRMS). This two-step method was applied to determine the δ¹³ C values of BDE-209 in two commercial samples and to characterize carbon isotope fractionation associated with the debromination of BDE-209 via nanoscale zero-valent iron.

Results:

The mean values of daily δ¹³ C analyses of six replicates of a BDE-209 standard varied from -27.66‰ to -27.92‰, with a standard deviation ranging from 0.07‰ to 0.16‰, indicating a good reproducibility of EA/IRMS. The EA/IRMS analysis of the purified BDE-209 standard indicated no obvious isotope fractionation during the sample purification. The impurity content in commercial BDE-209 samples may contribute additional variation of the δ¹³ C values of BDE-209. The δ¹³ C values of BDE-209 gradually changed from -27.47 ± 0.37‰ to -24.59 ± 0.19‰ when 74% of the BDE-209 standard was degraded within 36 h. The estimated carbon isotope enrichment factor was -1.72 ± 0.18‰.

Conclusions:

The two-step method based on HPLC and EA/IRMS avoids the thermal instability of BDE-209 in the traditional CSIA method. It offers a novel approach for elucidating the degradation mechanisms of BDE-209 in the environment and for source identification in contaminated sites.

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