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  • Title: Isolation and stable nitrogen isotope analysis of ammonium ions in ammonium nitrate prills using sodium tetraphenylborate.
    Author: Howa JD, Lott MJ, Ehleringer JR.
    Journal: Rapid Commun Mass Spectrom; 2014 Jul 15; 28(13):1530-4. PubMed ID: 24861604.
    Abstract:
    RATIONALE: Because of the threat of bombings using improvised explosives containing ammonium nitrate (AN), law enforcement and intelligence communities have been interested in stable isotope techniques for tracking and discriminating AN sources. Separate analysis of the AN component ions ammonium and nitrate would add discriminatory power to these techniques. METHODS: Ammonium ions in dissolved AN solution were isolated from samples by precipitation using sodium tetraphenylborate solution. We tested the isolation of ammonium from nitrates using solutions of ammonium and nitrate salts with different (15)N/(14)N isotope ratios. Ammonium tetraphenylborate and AN were separately analyzed for their (15)N/(14)N isotope ratios using EA-ConFlo-IRMS, and the (15)N/(14)N isotope ratios of the nitrate ions were calculated using mass balance. Ammonium and nitrate nitrogen isotope ratios were plotted as two separate variables. RESULTS: Isolation of ammonium precipitate from solutions containing dissolved nitrates did not influence the nitrogen isotope ratios of test ammonium salts. A survey set of 42 AN samples showed that the ammonium and nitrate (15)N/(14)N isotope ratios were not significantly correlated, and the paired mean differences were not statistically significant. Both ammonium and nitrate were depleted in (15)N relative to their theoretical atmospheric sources. CONCLUSIONS: Isolation of the ammonium ion from AN adds another dimension for the discrimination of forensic AN samples. This technique using sodium tetraphenylborate is robust and does not require specialized equipment. Our observations indicated that ammonium nitrogen and nitrate nitrogen have independent sources of isotopic variation.
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