62. to FEFO -e quite high (80 to 85%). The overall yield starting from VII, however, is 45 to 55s. <strong>and</strong> the large volumes <strong>and</strong> lengthy procedures,decrease the utility of this method even furthero Physical Characteristics of FEW FEFO is a colorless liquid, b.p. 120 to 124'C at 0.3 mm Hg,m.p. 14'C. Its density is 1.595 g/cc at 25'C. <strong>and</strong> its index of refraction n2$ = 1.4398. It is soluble in the lower aliphatic alcohols <strong>and</strong> esters, <strong>and</strong> in most chlorinated solvents. It is stable to strong acids, <strong>and</strong> relatively stable to dilute aqueous alkali. Its sensitivity to impact has given values ranging from 11 cm (5096 point, 2 Kg woight, RDX = 28 cm) to 40 to 50 cm (5& point, 2.5 Kg weight). Toxicity data are scanty but tend to indicate relstively lor toxicity, at least by external exposure to skin or eye. ,&alvais of FEPO Gas chromatography has been employed as the most suitable analytical method for FEFO assay. GC FEFO analyses are conducted <strong>with</strong> a six ring polyphenyl ether column <strong>and</strong> a sensitive flame ionization detector. A 2-minute isothermal run at 100°C is followed by a programmed increase of 6°C/minute to 20O0C, <strong>and</strong> an additional 8 minutes at 2CQ°C. All components are eluted <strong>with</strong>in a 20-minute period. These operating conditions give well-resolved peaks <strong>with</strong> minimal tailing. Although sample sizes have been varied between 0.2 <strong>and</strong> 0.8 ~l, 0.2 to 0.3 ul is preferred. Preliminary studies suggested that chromatograph oven temperatures between 180 <strong>and</strong> 20'C would not cause measurable decomposition of FEFO. Therefore, to enhance volatilization <strong>and</strong> peak shape, a pre-heater temperature of 185'C was selected. However, at this temperature the area percents of the mor. volatile components did not reproduce well, although consistent data were obtained for the other impurities. A later series of tests of vaporizer temperatures from 150 to 20O'C demonstrated the necessity of operating at 15OoC because of an apparent degradation of FEFO at the higher temperatures. Tho data suggest that the apparent increase in impurities of low retention time at temperatures above 15OCC is actually due to degradation of FEFO. Its assay decreases <strong>with</strong> the increase of these inpuritiea attendant <strong>with</strong> the increased temperatures. By operating the vaporizer at 15OoC, reproducible chromatograms are obtained <strong>with</strong>out noticeably altering the elution times. The anhydrous potentiometric titration applicable to FDNE may be used for TEFO also. FEPO can be titrated in acetonitrile <strong>with</strong> tetrabutylammonium hydroxide to give a single well-defined break corresponding to the removal of four protons per mole. A single sample assayed 08.816 FEFO, compared <strong>with</strong> 86.d obtained by gas chromatography. Since the impurities in FEFO are also apt to have acidic properties, this method was not developed further. Acknovledmm t The author wishes to expresa hie appreciation to Dr. M. J. Kanlet <strong>and</strong> Dr. 8. G. Adolph of the U.S. Naval Qrdnance Laboratory, White Oak, Maryl<strong>and</strong>, <strong>and</strong> to Dr. K. Baum, Dr. V. Crakauskas, <strong>and</strong> Dr. F. E. Nartin of the Aerojet-General Corpora- tion for pedasion to present cortain information prior to their own publications.
63. I 1. K. Klager, U.S. Patent 3,024,288 (1962). 2. v. GraKauskas <strong>and</strong> K. Baum, in press. I 3. K. Klager, J. P. Kispersky, <strong>and</strong> E. E. Hamel, J. Ora. Chm., &, 4368 (1961). I , 4. Irl. J. Kamlet <strong>and</strong> H. C. Adolph, J. Ora. Chem., in press. 5. Y. E. Martin, patent applied for. 6. K. C. Shipp <strong>and</strong> M. E. Hill, J. Ora. Chrm., 2, 853 (1966). 7. H. G. Adolph, private communication.
- Page 1 and 2:
Introduction 1. SECONDARY CELLS WIT
- Page 3 and 4:
I time curves at constant current d
- Page 5 and 6:
I 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11
- Page 7 and 8:
7. IV IV- Equivalent Weight, gr/ Eq
- Page 9 and 10:
1 3 9 SOYO FILLER,HQT PRESS Fig. 4.
- Page 11 and 12: 11. COAL PYROLYSIS USING LASER IRRA
- Page 13 and 14: 13. Macerals. Macerals from a singl
- Page 15 and 16: i 1 I Photochemistry. A fundamental
- Page 17 and 18: t P li. al ’ i ._ m LL
- Page 19 and 20: ' 19. PYROLYSIS OF COAL IN A MICROW
- Page 21 and 22: I 21. In the third stage, the gas e
- Page 23 and 24: .4 4 0 W 0 m .d m x .-( 0 x w M m s
- Page 25 and 26: ' 25. CONCLUSIONS The principal rea
- Page 28 and 29: ' .4 b s tract 28.
- Page 30 and 31: 30. the course of the experiment Ex
- Page 32 and 33: d (Sulfur] dt m i trogenj dt 32. E
- Page 34 and 35: 34. Table 1, Properties of Feed Mat
- Page 36 and 37: 0 0 0 m 0 VI b N 0 c, VI N 0 v, N h
- Page 38 and 39: - Literature Cited 38 1. Gordon, K
- Page 40 and 41: 40 z - B 30 w 6 20 yl w U 10 40. 10
- Page 42 and 43: Z 0 In 80 CK W > 6 60- 0 I- 40- Z W
- Page 44 and 45: 44. 2.0 I 1.2 - 0 2 1.0- 0.8 i TIME
- Page 46 and 47: - 2.81 1.NITROGEN 2. SULFUR 3. GASO
- Page 48 and 49: 48. The oil from the separator is v
- Page 50 and 51: . 50 . Table I . Properties of Pitc
- Page 52 and 53: 52. Coke yield A - - - - 0 800 900
- Page 54 and 55: FIGURE 8. 54. t 0.5 1 800 900 1,000
- Page 56 and 57: Introduction 56. FLUORODINITROETUNO
- Page 58 and 59: chloride extractant without other h
- Page 60 and 61: 60. identified (Reference 7) as the
- Page 64 and 65: 64. RECENT CHEMISTRY OF THE OXYGEN
- Page 66 and 67: polymers for the conventional fuel
- Page 68 and 69: 68. In summary, two general methods
- Page 70 and 71: 70. Table XI1 Differential Thermal
- Page 72 and 73: vapor Pressure (psia) Figure 4. Vap
- Page 74 and 75: C H -0-C-NHF, - 2 5 II 0 74. H 9304
- Page 76 and 77: 76. The infrared spectrum is descri
- Page 78 and 79: , 78. PREPARATION AND POLYMERIZATIO
- Page 80 and 81: . .- . - ..... . . I ,caving the re
- Page 82 and 83: If it ~ 3 ~ o~t 7 s Y'2t the therm1
- Page 84 and 85: Chlorine Fentafluaride T q D OC 252
- Page 86 and 87: , 86. Zeections of Cl30 and AsF5. M
- Page 88 and 89: aa . - The rrost difficult rctionel
- Page 90 and 91: 90. DENSITY, VISCOSITY AND SURFACE
- Page 92 and 93: 92. If it is assumed that the syste
- Page 94 and 95: 94. After condensation of oxidizer
- Page 96 and 97: Stirring Solenoid LHe 7. Cryostat 9
- Page 98 and 99: Introduction 98. RFACTIONS OF OxYcm
- Page 100 and 101: , Acknowledgement 100. This work wa
- Page 102 and 103: 102. volume and then by pumping to
- Page 104 and 105: 104. The x-ray powder pattern (Tabl
- Page 106 and 107: Irredie tion Time, mi&) 106. Table
- Page 108 and 109: I. Introduction 108. RE7IIEw OF ADV
- Page 110 and 111: 1.40 w F O/) 103-4O 'F 110. /H 0 21
- Page 112 and 113:
!P, "c -- -2118.5 -195 -172 -16.1 .
- Page 114 and 115:
114. weaker than those in NF02. The
- Page 116 and 117:
Compound C102F ~ 1 , 0 ~ -146 ~ 116
- Page 118 and 119:
118. fom such salts as cS+m8- have
- Page 120 and 121:
120. DETONABILITY TESTING AT NONAMB
- Page 122 and 123:
I 122. top) is closed with caps whi
- Page 124 and 125:
124. five pieces of MDF, each 20.00
- Page 126 and 127:
126. auxiliary equipment. For conve
- Page 128 and 129:
128. reliability. Details of most o
- Page 130 and 131:
130. The time required for the deto
- Page 132 and 133:
132. Fig. 2 Typical Witness Plate
- Page 134 and 135:
I ll 134. L, ALUMINUM 011+ ‘7 I-
- Page 136:
W (3 3 a (3 W m 3 0 v) W E k- / W 3