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A Photoionization Mass Spectroscopic Study on the Formation of Phosphanes in Low Temperature Phosphine Ices PCCP

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A Photoionization Mass Spectroscopic Study on the Formation of Phosphanes in Low Temperature Phosphine Ices PCCP Volume 17 Number 41 7 November 2015 Pages 27227–27902 PCCP Physical Chemistry Chemical Physics www.rsc.org/pccp ISSN 1463-9076 PAPER Agnes H. H. Chang, Ralf I. Kaiser et al. A photoionization mass spectroscopic study on the formation of phosphanes in low temperature phosphine ices PCCP View Article Online PAPER View Journal | View Issue A photoionization mass spectroscopic study on the formation of phosphanes in low temperature Cite this: Phys. Chem. Chem. Phys., 2015, 17,27281 phosphine ices† Andrew M. Turner,a Matthew J. Abplanalp,a Si Y. Chen,b Yu T. Chen,b Agnes H. H. Chang*b and Ralf I. Kaiser*a Isovalency rationalizes fundamental chemical properties of elements in the same group, but often fails to account for differences in the molecular structure due to the distinct atomic sizes and electron-pair repulsion of the isovalent atoms. With respect to main group V, saturated hydrides of nitrogen are limited to ammonia (NH3) and hydrazine (N2H4) along with ionic and/or metal-bound triazene (N3H5) and potentially tetrazene (N4H6). Here, we present a novel approach for synthesizing and detecting phosphanes formed via non-classical synthesis exploiting irradiation of phosphine ices with energetic electrons, subliming the newly formed phosphanes via fractionated sublimation, and detecting these species via reflectron time-of-flight mass spectrometry (ReTOF) coupled with vacuum ultraviolet (VUV) single photon ionization. This approach is able to synthesize, to separate, and to detect phosphanes as Received 16th May 2015, large as octaphosphane (P8H10), which far out-performs the traditional analytical tools of infrared Accepted 21st July 2015 spectroscopy and residual gas analysis via mass spectrometry coupled with electron impact ionization DOI: 10.1039/c5cp02835c that could barely detect triphosphane (P3H5) thus providing an unconventional tool to prepare complex inorganic compounds such as a homologues series of phosphanes, which are difficult to synthesize via www.rsc.org/pccp classical synthetic methods. 1. Introduction two members of main group V: nitrogen and phosphorus. Molecular nitrogen exists as a diatomic molecule (N2) in the 1 Ever since Langmuir devised the concept of isovalency in 1919, gas phase, while white phosphorus is composed of P4 tetra- this framework has presented a fundamental pillar of chemistry hedrons occurring in the liquid and gas phase and exists in Published on 05 August 2015. Downloaded by University of Hawaii at Manoa Library 14/10/2015 21:35:01. and elucidates the periodic property that elements in the same equilibrium with diatomic phosphorus (P2) at elevated tem- group with an identical valence electron configuration hold peratures above 1070 K.4 An evaluation of the molecular similar chemical properties. Isovalency has been exploited to structures of the hydrides of nitrogen and phosphorus demon- understand the chemical formulas, reaction mechanisms, strates simultaneously the validity, but also the shortcomings and even molecular geometries for a vast array of chemical of the isovalency concept. compounds. For instance, the molecular formulas for hydrides The two simplest azanes (NnHn+2; n = 1, 2) and phosphanes of main group V elements – ammonia (NH3), phosphine (PH3), (PnHn+2; n = 1, 2) have been known for more than a century. The arsine (AsH3), stibine (SbH3), and bismuthine (BiH3) – can be molecular formula of the most common and least toxic azane – 2 3 5 rationalized by the ns np valence electron configuration of the ammonia (NH3) – was determined in 1785 with phosphine 6 central atoms. However, factors related to the atomic radius as (PH3) being discovered in that same year. These were followed 7 well as bonding and non-bonding atomic orbitals have shown by diphosphine (P2H4) in 1844, which was surprisingly dis- to result in distinct molecular structures.2,3 These differences covered 50 years before its nitrogen analogue, hydrazine 8 are most evident considering the elemental forms of the first (N2H4). More complex molecules have proven to be more difficult to synthesize. Triazane (N3H5) was first reported as a 9 a Department of Chemistry, University of Hawaii at Manoa, Honolulu, silver-complex and later monitored via its molecular ion Hawaii 96822, USA. E-mail: [email protected]; Tel: +1-808-956-5731 exploiting microwave plasma discharge of hydrazine.10 This b Department of Chemistry, National Dong Hwa University, Shoufeng, Hualien 974, study tentatively characterized tetrazane (N4H6), but only as a Taiwan. E-mail: [email protected] † Electronic supplementary information (ESI) available: Calculations and diagrams complex with lithium. Thus, free azanes heavier than hydrazine used to determine the refractive index of phosphine, the experimental ice thickness, have been difficult to synthesize and require a metal–cation and integrated absorption coefficients. See DOI: 10.1039/c5cp02835c complex to stabilize the molecule in the gas phase or in zeolites. This journal is © the Owner Societies 2015 Phys. Chem. Chem. Phys., 2015, 17, 27281--27291 | 27281 View Article Online Paper PCCP Despite the isovalency between nitrogen and phosphorus, far temperature was chosen to minimize thermal chemistry in the larger hydrides of phosphorus have been detected.11 Triphosphane ice. Reflectron time-of-flight (ReTOF) mass spectroscopy coupled (P3H5) was first probed via Ramanspectroscopyasatransient with ‘soft’ single vacuum ultraviolet (VUV) photon ionization at species12 and was also isolated for preparative studies.13 Heated 10.49 eV is applied to explicitly identify the molecular formulas of mixtures of diphosphine (P2H4) and triphosphane (P3H5)produced the newly synthesized phosphanes on line and in situ upon their traces of tetraphosphane (P4H6), which could not be purified due sublimation into the gas phase upon warming of the irradiated to rapid disproportionation. Further heating lead to the formation of poorly defined mixtures of pentaphosphane (P5H7), hexaphos- phane (P6H8), and heptaphosphane (P7H9), which could not be separated due to the thermal instability of higher phosphanes. Octaphosphane (P8H10) and nonaphosphane (P9H11)wereonly identified tentatively.11 The fact that phosphorus can form more complex hydrides than nitrogen illustrates that additional factors beyond isoelectronicity affect the chemistry of these elements, such as the established tendency of nitrogen to favor the formation of multiple bonds due to the smaller radius of the nitrogen atom (71 pm) compared to phosphorus (109 pm).14 However, despite the tentative identification of higher phosphanes, their underlying synthetic pathways together with their explicit isolation and pro- tocols to their clean preparation have not been established to date. Here, we demonstrate that phosphanes up to octaphosphane (P8H10) can be efficiently prepared and thereafter separated via fractionated sublimation upon exposure of phosphine ices to energetic electrons at ultralow temperatures of 5.5 K. The low Table 1 Infrared absorption assignments for phosphine ice at 5.5 K and the products of electron irradiation Assignmenta Position (cmÀ1) Phosphine ice, pre-irradiation (5.5 K) n2 (d(HPP)) 983 n4 (d(HPP)) 1097, 1108sh n2 + n4 2067, 2083 2n4 2195 n1 (n(PH)) 2303 n3 (n(PH)) 2316 n1/n3 + nL 2376, 2426, 2461 Published on 05 August 2015. Downloaded by University of Hawaii at Manoa Library 14/10/2015 21:35:01. 3n2 2905 n1 + n2 3288 n1 + n4 3392 Fig. 2 (Top) Overlay of infrared spectra of solid PH3 taken before (dashed n3 + n4 3405 line) and after (solid line) irradiation, with the spectrum after PH sublimed 2n1 4536 3 n1 + n3 4621 (85 K, dotted line) emphasizing the products of irradiation. The inset expands the lower intensity region from 1200–900 cmÀ1. (Center) Infrared New peaks from irradiation spectra of the P–H stretching region after PH3 (85 K, dotted line), P2H4 n d P2H4 ( 11, (HPP)) 1061 (130 K, dashed line), and P3H5 (165 K, solid line) sublime. (Bottom) Infrared P2H4 (n5, n(PH)) 2294 spectrum of P H obtained by subtracting the post-P H sublimation n 3 5 3 5 P3H5 ( (PH)) 2264, 2288 spectrum from its pre-sublimation spectrum. The peaks at 2264 cmÀ1 P H (d(HPP)) 1059 3 5 and 2288 cmÀ1 (left) result from P–H stretching while the peak at a Assignments based on previous studies.43,44 1059 cmÀ1 (right) corresponds to H–P–P bending. Fig. 1 Infrared spectrum of pre-irradiated solid phosphine taken at 5.5 K. 27282 | Phys. Chem. Chem. Phys., 2015, 17, 27281--27291 This journal is © the Owner Societies 2015 View Article Online PCCP Paper target to 300 K. Our study presents clear evidence of higher 2. Experimental section molecular mass phosphanes thus providing a clean route to their formation up to octaphosphane (P H ) via exposure of phos- The experiments were conducted in a contamination-free ultra- 8 10 À11 phine ices to energetic electrons followed by fractionated sub- high vacuum stainless steel chamber evacuated to a few 10 limation of the phosphanes. This study further provides a proof Torr using oil-free turbomolecular pumps and dry scroll back- 15–24 of concept for a novel adaption of ReTOF mass spectroscopy ing pumps, which has been described previously. Briefly, a coupled with VUV single-photon ionization to form and to silver mirror substrate is mounted onto a rotatable cold finger identify inorganic molecules, which are difficult to synthesize made of oxygen-free high-conductivity copper (OFHC) cooled to via classical synthetic methods. 5.5 K Æ 0.1 by a closed-cycle helium refrigerator (Sumitomo Heavy Industries, RDK-415E). Phosphine
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