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Interim Report on the Thermodynamics of Chemical Species

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Interim Report on the Thermodynamics of Chemical Species A FOSR Scientific Report D_A DITMARS (gS) A FOSR— TR — 72— 2004 NATIONAL BUREAU OF STANDARDS REPORT 10 904 INTERIM REPORT ON THE THERMODYNAMICS OF CHEMICAL SPECIES IMPORTANT IN AEROSPACE TECHNOLOGY (including Special Topics in Chemical Kinetics) (The previous reports in this series have the NBS Report Nos. 6297, 6484, 6645, 6928, 7093, 7192, 7437, 7587, 7796, 8033, 8186, 8504, 8628, 8919, 9028, 9389, 9500, 9601, 9803, 9905, 10004, 10074, 10326, and 10481.) Y U.S. DEPARTMENT OF COMMERCE NATIONAL BUREAU OF STANDARDS This document has been approved for public release; its distribution is unlimited. Qualified requestors may obtain additional copies from the Defense Documentation Center. All others should apply to the National Technical Information Service. NATIONAL BUREAU OF STANDARDS REPORT MBS PROJECT MBS REPORT 232-0423 1 July 1972 10 904 316-0401 316-0403 3 16-0405 316-0426 INTERIM REPORT ON THE THERMODYNAMICS OF CHEMICAL SPECIES IMPORTANT IN AEROSPACE TECHNOLOGY (including Selected Topics in Chemical Kinetics) (The previous reports in this series have the NBS Report Nos. 6297, 6484, 6645, 6928, 7093, 7192, 7437, 7587, 7796, 8033, 8186, 8504, 8628, 8919, 9028, 9389, 9500, 9601, 9803, 9905, 10004, 10074, 10326, and 10481.) Reference: U. S. Air Force, Office of Scientific Research, Agreement No. A F OSR — ISSA — 71 — 0003, Project No. 9750-01 <NBS> U.S. DEPARTMENT OF COMMERCE NATIONAL BUREAU OF STANDARDS CONDITIONS OF REPRODUCTION Reproduction, Translation, publication, use and disposal in whole or in part by or for the United States Government is perm itted. FOREWORD Structure, propulsion, and guidance of new or improved weapons delivery systems are dependent in crucial areas of design on the avail- ability of accurate thermodynamic data. Data on high-temperature materials, new rocket propellant ingredients, and combustion products (including exhaust ions) are, in many cases, lacking or unreliable. This broad integrated research program at the National Bureau of Standards supplies new or more reliable thermodynamic properties essential in several major phases of current propulsion development and application. Measured are compounds of those several chemical elements important in efficient propulsion fuels; those substances most affecting ion concen- trations in such advanced propulsion concepts as ion propulsion; and the transition and other refractory metals (and their pertinent compounds) which may be suitable as construction materials for rocket motors, rocket nozzles, and nose cones that will be durable under extreme conditions of high temperature and corrosive environment. The properties determined extend in temperature up to 6000 degrees Kelvin. The principal research activities are experimental, and involve developing new measurement techniques and apparatus, as well as measuring heats of reaction, of fusion, and Q f vaporization; specific heats; equilibria involving gases; several properties from fast processes at very high temperatures; spectra of the infrared, matrix-isolation, microwave, and electronic types; and mass spectra. Some of these techniques, by relating thermodynamic pro- perties to molecular or crystal structures, make it possible to tabulate reliably these properties over far wider ranges of temperature and pressure than those actually employed in the basic investigations. Additional research activities of the program involve the critical review of published chemical-thermodynamic (and some chemical-kinetic) data, and the generation of new thermochemical tables important in current chemical-laser research. i ABSTRACT This report presents recent results of the NBS research program. The nature and scope of the subjects covered may be inferred from the detailed Table of Contents to be found on the following pages. The most significant results may be summarized as follows, under four main headings. (1) Thermodynamic properties of molybdenum compounds -- As a necessary preliminary to later measurement of the standard heat of formation of M0F that of MoFg was determined by solution 3 , (f) calorimetry and found to be AHf° = -376.43 ± 0.52 kcal mol"l. The related standard heat of formation of F“(aq) and heat of solution of NaF(c) are discussed critically. Fifteen new transpiration measure- ments on MoF^(^) at 70°, 90°, and 110°C are reported. To enable determination of the individual partial pressures of monomer and dimer vapor species, a second vapor-pressure method was developed which reproduced known vapor pressures of iodine to within 1 to 2%. Assuming the M0F molecule to have symmetry, a complete vibrational assign- 5 03 ^ ment was made on the basis of new studies (infrared spectra of the matrix- isolated vapor, using double-boiler techniques to enhance the monomer; and Raman spectra of the crystal and the liquid) . The heat capacity of what is approximately M02 C was measured from 273 to 1475 K using two drop-type calorimeters; these results are consistent among themselves and with two published low-temperature heat-capacity sets of data, and extension of the measurements to well above a first-order transition (at about 1675 K) is planned. (2) Thermophysical properties of refractory metals and alloys --The subsecond -duration pulse-heating technique previously developed and applied was used to measure simul- taneously the specific heat, electrical resistivity, and hemispherical total emittance of two alloys, Ta-10(weight %) W(1500-3200 K) and Nb-l(weight %) Zr (1500-2700 K), with estimated accuracies comparable to those obtained on other samples previously. The specific heats show small departures from the additive values based on the pure components. The electrical resistivity of the former alloy shows significant departure from Mattiessen's law, and that of the latter alloy is 0.5% lower than for pure Nb. The pulse-technique melting point of W was found to be 3695 K, and that of Nb, 2750 K (both IPTS- 68), with estimated uncertainties of 15 K and 10 K, respectively; the electrical resistivities of both metals also were measured above their melting points, and the normal spectral emittance of Nb remained constant at 0.348 (±3%) during melting. The feasibility of a pulse-heating technique for measuring the heats of fusion of refractory metals was demonstrated by preliminary experiments on Nb ; and the feasibility of another such technique for solid-solid phase transformations at high temperatures was demonstrated by the rate of surface radiance-temperature variation in the gamma-to-delta transformation of Fe, during which the electrical resistivity increased by 0.3%. (3) Chemical kinetics of simple-gas reactions --On the basis of a critical examination of the data (especially shock-tube), suggested thermal rate constants are tabulated for the six iii dissociation and recombination reactions (a) NH~ ** NH., + H (0-100 atm, -5 and 200-4000 K) (b) N H, - 2NH -100 atm, and 200-3000 K) and , 2 2 (10 , (c) N F^ ^ 2NF (10"5 -100 atm, and 200-1800 K) . The best fit of (a) 2 2 appears to require external rotation. A satisfactory data correlation of (b) was made using RRKM unimolecular rate theory, and the results are consistent with AHf = 45.5 ± 1.5 kcal mol”-®- for NH (in- 2 gg 2 (g) corporated in a new thermochemical table) instead of the JANAF-table value of 40.1 ± 3. The RRKM data correlation of (c) requires 18.0 kcal (0 K) for the N-N bond energy (JANAF value, 20.8 kcal). In addition, a bibliography (1934-June 1972) covers the chemical kinetics of 60 gas-phase reactions of fluorides of C^, N, and 0 based on 51 papers, with emphasis on the processes occurring during the thermal decompositions of these fluorides. (4) New ideal-gas thermo chemical tables- -Based on a critical review and correlation of the up-to-date heat-of -formation and molecular-constant data, new ideal-gas thermo chemical tables and texts of the JANAF-Table format are given for 31 simple gas species containing H (or^H), D (or ^H), F, C^, 0, S, and/or N. Included are (HF) with n = 1 to and texts (but no tables) for F and H 0. n 7, 2 2 TABLE OF CONTENTS Page Foreword . i Abstract iii Chap. 1. THE HEAT OF FORMATION OF MoF (&) BY SOLUTION CALORIMETRY (by R. L. Nuttall, K. L. Churney, and M. V. Kilday) 1 1. Introduction 1 2. Reaction Scheme of Solution Experiments 4 3.0. Materials 5 3.1. Sample Bulbs for MoF^(L) 6 3.2. Calorimeter ..... 7 3.3. Experimental Procedures 8 4. Experimental Results 10 4.1. Reaction (2) 10 4.2. Reaction (3) 13 4.3. Reactions (4) and (5) . 13 Reaction (7) 14 8. Discussion of Results 14 8.1. Enthalpy of Formation of MoF,(£) and F (aq) . 14 8.2. Heat of Solution of NaF(c) 17 References 18 Table 1. Calorimetric Data for Reaction (2) 20 Table 2. Drift Rate Data for Reaction (2) 21 BA 22 Table 3. Calculation of . Table 4. Calorimetric Data for Reaction (3) 23 Table 5. Calculation of /H3 24 Table 6. Calorimetric Data for AH4 (Set 5) and AH5 (Set 6 ) ........ 25 Table 7. Calculation of AH4 26 Table 8. Calculation of /H5 27 Table 9. Calculation of AH7 28 Chap . 2 . MOLYBDENUM PENTAFLUORIDE : VAPORIZATION PROPERTIES FROM TRANSPIRATION , AND DEVELOPMENT OF AN EXPERIMENTAL METHOD TO EVALUATE THE TRUE VAPOR PRESSURES (by Thomas B. Douglas and Ralph F. Krause, Jr.) 29 Abstract ...... ..... 29 I. Introduction 29 II. Transpiration Measurements 30 1. Experimental Results 30 Fig. 1. Transpiration apparatus 32 Table 1. Transpiration of MoF,-(£) by Helium Containing MoF^(g) 33 v TABLE OF CONTENTS (Continued) Page 2. Concerning the Molecular Weight of Molybdenum Pentaf luoride in the Vapor State 35 Fig. 2. Deviations of the results1 of indi- vidual experiments from Equation (2) 36 III. Development of a Method to Measure the True Vapor Pressures 39 1. Brief Description of the Method 39 2. Apparatus Design and Experimental Procedure. 40 Fig. 3.
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