ORNL-1771 - Oak Ridge National Laboratory

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This procedure, which is simple, rapid, and capable of high internal precision, yielded the values plotted as the lower curve in Fig. 5.7. The logarithm df the HF concentration is plotted against the logarithm of the FeF, concentration at various flow rates of hydrogen. When these values are corrected to the “zero flow rate” (9 rnl/min) by io2 2 5 4 o3 2 CONCENTRATION OF FeFz (ppm Fetf) PERIOD ENDING SEPTEMBER 70, 1954 reference to Fig. 5.6, they yield a consistent straight line after an initial peak. This initial peak is probably due to the reaction of HF at its initial high concentrations with the clean (hydrogen-fired) nickel apparatus and its subsequent re-equilibration with the more dilute HF-H, mixture. The straight- line portion of the curve shows the expected slope UNCLASSIFIED <strong>ORNL</strong>-.LR-DWG 2927 5 1 o4 Fig. 5.7. Equilibrium Concentration for the Reduction of FeF, by H, in NaF-ZrF, (53-47 mole %) at 800°C (Obtained by Dynamic hethod). 65
ANP QUARTERLY PROGRESS REPORT of 0.5 and agrees closely with the slruiyht line calculated from Brewer’s value of AFa for the reaction. The values obtained for Kx and for Y F ~ on F ~ the assumption that the activities of HF and W, are proportional to their partial pressures at 8OOOC and that and Al:OFeF2 - -45.4 kcal per atom of F LIFO,, = -65.8 kcal per atom of F are shown in Table 5,7, The QgiYXment of the values obtained over CI fourfold concentration runge of FeF, is extremely good. It appears that FeF, in molten NaF-ZrFd is in nearly ideal solution. TABLE 5,s. EQUlLlBRlUM CONSTANTS AND ACTiVlTY COEFFICIENTS AT 800OC IN MQLTEN NcsF-ZrF4 (53-47 mole X) FOR THE REACTiOW H2 t FeF2eFeo + 2HF 1598 1513 1458 1372 1318 1233 1122 1067 983 900 8 57 760 606 5.50 48 1 2.15 2.15 2.17 1.98 1.91 2.37 2.07 2.00 2.11 2.18 2.11 2.17 2.19 2.24 2.19 Av 2.13 f 0.22 1.47 1.47 1.48 1.36 1.3 1 1.62 1.38 1.37 1.44 1.49 1.45 1.49 1.50 1.S4 1.50 1.46 f 0.16 Equilibration Method. Since it was doubtful that the lowest flow rate found to be practicable (9 ml/min) actually represented equil ibriurn conditions, an attempt was rnode to determine the equilibrium conditions directly. A mixture of HF and H2 was bubbled through a melt containing Fao and FeF, until the influent HF concentration matched 66 thot of the effluent. At that time a sample was drown through a sintered nickel filter and analyzed to determine the FeF, concentration. Since the decomposition pressures of molten KFaHF saturated with KF depend only on temperature,19 definite mixtures of H, and HF could be obtained while hydrogen gas WQP passed over such mixtures held at a constant temperature. The mixtures of H, thus obtained were used as influent for the reactor containing the salt mixture. In a typical experiment in which this method was used, a batch (“3 kg) of previously purified NaF- ZrF, (53-47 mole %) mixture WQS loaded into a clean nickel reactor. The mixture was heated to 80OoC and further puiified with hydrogen until a very low HF concentration (“3 x mote/Iiter) in the effluen* gas denoted high purity of the melt. The mixture vias allowed to cool to roam temperature, and FeF, and iron wire wereadded to the cold, frozen mixture under un atmosphere of argon. The mixture was then heated, melted, and brought up to temperature while it was sparged with helium gas. The reactor containing the KF*HF or HF generator SVQS heated separately to a convenient initial temperature and connected to the system. Pure hydrogen was passed in parallel through both reactors - the HF geiuerator and the equilibration reactor - in order to clean out any NiF, films on vmlls and to precipitate nickel impurities. After 1 to 2 hr of parallel operation, the reactors were connected in series, and the inlet on$ effluent gas streams were continuously sampled and analyzed. The temperature of the furnace of the generator was then adjusted until the analyzer showed H,-HF mixtures of the desired composition. The gas mixture was allowed to bubble through the system for extended periods of time, and samples were taken intermittently for analysis. When it was considered that the system had approached equilibrium, as indicated by a convergence of the influent and effluent compositions, the HF generator was removed from thz systern and helium was substituted for the influent gas mixture. A filtering tube was introduced into the melt under an additional argon atmosphere and a filtrate was obtained. The filtering tubs with the frozen filtrate was removed and analyzed for iron. This procedure was repeated with appropriate variation of the temperaturf: of the HF generator and consequent variation of the influent gas composition, 19G. H. Cndy, /. Am. Chern. SOC. 56, 1432 (1934).
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Contract No. W-7405-eng-26 AIRCRAFT
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1. G. M. Adamson 2. R. G. Affel 3.
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197-198. Powerplant Laboratory (WAD
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FOREWORD This quarterly progress re
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PART II . MATERIALS RESEARCH 5 . CH
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Remote Metallography ..............
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ANP QUARTERLY PROGRE.S.5 REPORT ver
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AMP QUARTERLY PROGRESS REPORT A dev
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part I REACTOR THEORY, COMPONENT DE
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AMP QUARTERLY PROGRESS REPORT After
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ANP QUARTERLY PROGRESS REPORT the A
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Page 42 and 43: Power level TABLE 2.6. COMPARISON O
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ANP QUARTfRLY PROGHESS REPORT As be
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ANP QUARTERLY PROGRESS REPORr Devel
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ANP QUARTERLY PROGRESS REPORT UNCL
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ANP QUARTERLY PROGRESS REPORi UNCLA
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ANP QUARTERLY PROGRESS REPORT lncon
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ANP QUARTERLY PROGRESS REPORT Fig.
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ANP QUARTERLY PROGRESS R€PORT 450
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ANP QUARTERLY PROGRESS REPORT TABLE
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132 ANP
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ANP QUr4RTERLY PROGRESS REPORT Addi
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ANP QUARTERLY PROGRESS REPORT mater
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ANP QUARTERLY PROGRESS REPORT 138 (
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ANP QUARTERLY PROGRESS REPORT Fig.
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ANP QUARTERLY PROGRESS REPORT The c
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ANP QUARTERLY PROGRESS REPORT oxide
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ANP QUARTERLY PROGRESS REPORT - n 6
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ANP QUARTERLY PROGRESS REPORT 10. A
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ANP QUARTERLY PROGRESS REPORT Oxide
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ANP QUARTERLY PROGRESS REPORT and U
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zirconium or aluminum complex, or l
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11. SHIELDING ANALYSIS J. E. Faulkn
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form in terms of the Spence functio
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these integral 5 become Let and the
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PERIOD ENDING SEPTEMBER IO, 7954 Al
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0 20 40 60 80 IO0 120 140 160 I, Di
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... Two configurations, a single du
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The thermal-neutron flux (Fig. 13.2
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E-7 1 O6 I 5 - - L I ___- 2 f o5 2
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TIME (rnin) PERIOD ENDING SEPTEMBER
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. - ., . ....._____... - PERiOD END
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io3 5 .--w 2 _J U 0 0 >- " 2 2 40 t
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PERIOD ENDING SEPTEMBER 10, 1954 Fi
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part IV APPENDIX
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REPORT NO. ~~-54-a-10 C F-54-6-4 CF
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