TY - JOUR
T1 - Characterization of bis(alkylamine)mercury cations from mercury nitrate surfaces by using an ion trap secondary ion mass spectrometer
AU - Groenewold, Gary S.
AU - Appelhans, Anthony D.
AU - Ingram, Jani C.
N1 - Funding Information: The funding support of the U. S. Department of Energy, Office of Technology Development, and Lockheed Martin Idaho Technologies Corporation, is gratefully acknowledged. The assistance of A. K. Gianotto in the preparation of the figures manuscript is also gratefully acknowledged.
PY - 1998/1
Y1 - 1998/1
N2 - Mercury-cyclohexylamine (R-NH2, where R = c-C6H11) ions having the composition Hg(R-NH)2H+ can be formed by exposing the surface of Hg(NO3)n=1,2 salts to gaseous primary amines and then sputtering the surface with a primary ion beam (ReO-4). The resultant ions can be stabilized and detected using an ion trap secondary ion mass spectrometer (IT-SIMS) instrument, which provides collisional stabilization that facilitates their observation. Isolation of the Hg(R-NH)2H+ ions followed by collisional activation produces daughter ions corresponding to (C6H10NH2)+and Hg(R-NH)+. These assignments were supported by deuterium labeling experiments, which resulted in the formation of Hg(R-NH)(R-NH-d11)H+ and Hg(R-NH)2H+. The existence of the Hg(R-NH)2 compounds on the surface was verified using Raman spectroscopy, which showed a strong absorption at 590 cm-1 that corresponded to Hg-N stretching. Analogous ions could be formed with n-hexylamine, but no Hg-bearing ions were formed when starting with a secondary or a tertiary amine. This indicates that only primary amines will react with Hg-nitrate surfaces in this manner. Hg-amine ions could not be formed starting with other Hg salts: chloride, iodide, thiocyanate, sulfate, and oxide. These results suggest that surface derivatization using amines, coupled with an IT-SIMS instrument, may offer an approach for determining inorganic metal speciation on surfaces. (J Am Soc Mass Spectrom 1998, 9, 35-41)
AB - Mercury-cyclohexylamine (R-NH2, where R = c-C6H11) ions having the composition Hg(R-NH)2H+ can be formed by exposing the surface of Hg(NO3)n=1,2 salts to gaseous primary amines and then sputtering the surface with a primary ion beam (ReO-4). The resultant ions can be stabilized and detected using an ion trap secondary ion mass spectrometer (IT-SIMS) instrument, which provides collisional stabilization that facilitates their observation. Isolation of the Hg(R-NH)2H+ ions followed by collisional activation produces daughter ions corresponding to (C6H10NH2)+and Hg(R-NH)+. These assignments were supported by deuterium labeling experiments, which resulted in the formation of Hg(R-NH)(R-NH-d11)H+ and Hg(R-NH)2H+. The existence of the Hg(R-NH)2 compounds on the surface was verified using Raman spectroscopy, which showed a strong absorption at 590 cm-1 that corresponded to Hg-N stretching. Analogous ions could be formed with n-hexylamine, but no Hg-bearing ions were formed when starting with a secondary or a tertiary amine. This indicates that only primary amines will react with Hg-nitrate surfaces in this manner. Hg-amine ions could not be formed starting with other Hg salts: chloride, iodide, thiocyanate, sulfate, and oxide. These results suggest that surface derivatization using amines, coupled with an IT-SIMS instrument, may offer an approach for determining inorganic metal speciation on surfaces. (J Am Soc Mass Spectrom 1998, 9, 35-41)
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U2 - 10.1016/S1044-0305(97)00231-6
DO - 10.1016/S1044-0305(97)00231-6
M3 - Article
SN - 1044-0305
VL - 9
SP - 35
EP - 41
JO - Journal of the American Society for Mass Spectrometry
JF - Journal of the American Society for Mass Spectrometry
IS - 1
ER -