chemical physics of discharges - Argonne National Laboratory

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418 cual. A mjor aa\;antage or' the bf6ssbauer technique is that the iron is observed without alteri:ig its chemical state or eniiiroluuent. The relatively low atonic nilnber Oi' the mjor deinents present :Bakes it possible for small: amounts of iron to >e obser.;ed in rather large amoun':,s 01' cml. Sa:nples of whole coal and vitmin as free as 2ossible from ninerals xere selected in wder to iyiinimize mineral-iron interzerence, and a I'ew saiqles vhose chemical analysis indicated "organic" iron were included. I ES'ERIMENTAL PROCEDURES Nine specixens, yritrain or vhole-coal, of seven coals with rank from lignite (72:. C) to anthracite (93;: C) were ased. Their designations and geographic origins are given in Table 1, in order of increasing carbon content. Table 2 is a compilation of the analytical data for C, H, N, S, Fe, ash, and 0 (by difference) on samples of these materials, as determined by the Coal Analysis group at the Bureau of Mines. The total iron in the coal was determined by ash analysis. HC1-soluble iron was determined by treating a separate powdered sample with 23;; HCl to extract any iron present as carbonates, oxides, sulfates, etc. Pyrite iron was then removed by treating the HC1-leached coal with 25;; €IN& to dissolve the iron conbined with sulfur; the extract was evaporated to dryness to expel oxides of nitrogen, and the residue was dissolved in HC1. In each case the iron was reduced with SnC12, the slight excess of which was eliminated with HgC12. "he reduced iron was titrated with potassium dichromate. "Organic" iron was then calculated by subtracting the two acid-soluble iron contents from the total iron. The Zesulting iron contents are listed in Table 2 as: total, HC1-soluble, pyrite, and organic . MEssbauer spectra were obtained on coal samples that were ground in a mortar and pestle. A cylindrical cell, open on one end with a circular aperture of 7.14 em2, was made by gluing a sheet of lucite 1/52" thick with Duco cement to the bottom of a circular wall mde from a paper card. A 3.50-g sample was then placed into this cell. The top window, also 1/32" lucite, was then cemented in place. The sample mass per unit area was thus held oonstant at 0.4% g cmm2. Inorganic iron compounds and mineral samples were ground and mounted either between two lucite sheets held together with Duco cement, or by mixing the solid with acetone and Duco cement and alluwing this mixture to harden on a lucite sheet. This latter method was used only when the sample would not interact with acetone or the cement. The area for these samples was also 7.14 cm2. All of the materials used in this investigation contained natural iron with presumably 2.19 atom $ FeS7. The M'dssbauer spectrometer incorporates a Nuclear Science and Engineering Corporation Model-B lathe-type drive modified in this laboratory for automatic operation. The operating mode employs constant velocit advanced in increments of C.05 mm s-'. The detector of the 14.4-kev Co57 -. Fegf gamm radiation is a Reuter-Stokes proportional tube containing lo$ methane in krypton, feeding through a single-channel analyzer set at 11 - 17 keV. Absorbers were mounted on the moveable table pe endicuLar to the radiation beam. The stationary source consists of - 5 di of co5Fdirfused into chromium metal. A Bird-Atcrmic scanning count integrator and Varian chart recorder plot the number of counts in a constant time interval at each velocity in succession. Powdered samples of sodium nitroprusside gave an isomer shift, relative to the CoS7-Cr source, of -0.11 mm s-l, and a uadrupole splitting of 1.68 m &I-'. With this source a line width of 0.25 mm s-' was obseNed with an absorber containing 5 ny cmS of Fe as K4Fe(CN)e.3&0. The estimated uncertainty in the velocity setting is about 2: of the velocity and the estimated uncertainty in derived spectral parameters is - 0.05 mm sL. The counting time at each velocity was - 5
I n \D r- m d c d rl rl n . aJ 2 C W c, d X . a d t- 0 2 Po .> E. r: . 2 c, d > r: aJ c, E d PI ? ? 0 0 no\ (d' ? 5 P d F O x n (v k 4 2 d u 0 c, c I1 ?I t
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)i 1 reesonably complete and accura
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3 inquire about the component of ve
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4 I I 5 To find (t2)av, we assume t
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\ vnich, it is noted can be negativ
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I 7 than or smaller than the second
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i I i I I I ) ) i L , I I . INT1:OD
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13 field per electron is and per co
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. 11. 5. CharRe-Transfer and Ion-Mo
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17 In the followin:: sections much
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above. With that EIN, an estimate o
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21 region in w!iich large, nighlv l
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i ’ understanding: 23 (a) Electro
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Obviously, the secondary ion must h
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27 (22) Franklin, J. L., Munson, M.
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Tables 1-6 present examples of rela
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Table 8 Some Ions Formed by Process
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33 velocity of the reacting partn r
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35 must be added to the Langevin cr
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37 In our laboratory a microwave di
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+ . 4 . r 39 as well as N in a cor0
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ION-MOIECULE REACTION RATES MEASUFI
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43 excitntion 2onditions so that th
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45 In 2 like manner Fig. 3, showing
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47 Absorption Spectra of Transient
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50 maximum fiela. In this manner, a
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52 3 % %- %- 5- a- 7 h W P H 0 L v)
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References I I . A.B.Callear, J.A.G
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._ . _-.. - , , . . ,. . The Pyrex
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58 0 0 0 VI J > I cv . u H a
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.... . 0 2 e I / m 0 H F4 : 1
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\ 0.9 0.8 0.7 06 0.5 0.4 0.3 0.2 01
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65 ' cause of the reduction in the
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INTRODUCTION I' Attachment of polar
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I 69 EXPERIMENTAL The mass spectrom
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+ Figure 1 Mixed water and methanol
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73 ' , radius might be expected bec
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75 Negative Ion Mass Spectra of Som
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A b 1 1 I H I I I FILAMEN T CONTINU
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79 for positive and negative ions,
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51 out to answer some of the questi
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93 INTERACTIONS OF EXCITED SPECIES
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L 4 I*C z 0'2 = a, a U x I m 4 m 0
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I L I, ; > > E Fig. 3 I50 200 150 1
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I 300 r 1 - 200 i io ;' a cn I I. 0
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where DISCUSSION OF XESULTS PERTAIN
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93 where the bar indicates values c
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'I i 'I 0 2. 4 6 8 2 [ N]* x' I 0-2
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Fig. 14 IO 8 6 4F [NO] x IO-" (mole
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for chemiluminescent excitation in
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101 Chemiluminescent Reactions of E
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103 All gases were taken directly f
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10; He: + N2 -. 2He + h': (8) whi!?
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description for both diffusion and
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B. Ions and Electrons I Consider a
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' 112 axial diffusion through the d
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the tube walls occurs continuously
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E2R M ' $6"
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1. 2. 3. 4. 5. 6. 7. 8. 9- 10. u. -
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120 . Dlschorge zone Reactor zone 1
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122 In radiation chemistry the cust
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124 4. chemistry seem limited essen
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126 Conversion of Mixtures into Mor
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Hydrazine Synthesis in A Silent dle
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{;I . - . .. . - .., . . .. _- .. .
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1 \ \ \ , \ , \ \ Pmer hnrity K.W.
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. I operating fact that the sloGe i
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_- of ' . 8. - 7 6, Residence Time
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135 Ionic Reactions in Corona Disch
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GAS OUT GAS IN i.ho QUADRUPOLE MASS
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- + ( ~ ~ + 0 H ) ~ O ~ ( H~o)~H+ +
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144 i I , , , , . + 1- u 3c w Inu c
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146 SYNTHESIS OF ORGANIC COIGhTDS B
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mi5 a- dz CI n I a I n +4 - 0 -I- k
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0 z cu I I I
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I- I - t d m a .rl Y x c, t-' d k
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, 155 This result is significant in
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Compound Bond he rgy Li I 82 UBr 10
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, ”..’ 3or 25 - 5 20 - s 3 w Y
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I 161 THE GLOW DISCHARGE DEPOSITION
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Fig. 1 Process Apparatus -__l.ll__
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v) t- at- InIo Io0 t-Q) loo lcua O
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This study is only an approximation
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Mole Reaction Material ratio time e
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\ i (4) Effect of System Pressure T
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173 Pressure. Since pressure is a c
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175 Table VI X-RAY DATA OF DEPOSIT
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177 Another source of weakness is t
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179 PLATING IN A CORONA DISCHARGE R
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\ 3 , ,\ 110 v 60 CPS MANOMETER . F
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I i , \ I i & a - P Fig. 3 Reaction
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\ \' C 0 .d * d .- C U d 0) c( 1) L
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I i I . Q) I, s w 0 v) Y 0 a w W a
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I (b) Polarized Light Fig. 6 Cross
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i m v) Y C i! u o) 23 a a- + 191 m
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i, d C .d c c W Q ) 0 0 L1Y 0 000 0
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i e 4 0 wcr -4 4 al 0 0 0 c) cr 13:
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\ E ‘ 1 TIME FOR RUN 13-1 14-1 -
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199 a red heat in this cell using d
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\ , t j \ I, v) 2 Y . C 0 u m .I C
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203 VAPOR PHASE FORMATION OF NONCRY
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BELL JAR STANC TO VACUUM SYSTEM U T
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207 of the boron oxide film, the fi
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i I, 4 I.( Y I- * 0 i f i 3 0.t I I
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211 The Reacticn 3f Oxygen with Car
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2 E, W t- a Z 9 I- a 2 X 0 I50 too
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'i' 100 50 IC 21 5 2.0 2.5 SURFACE
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I- z W 0 w a a 100 80 60 40 20 215
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s., Literature Cited Berkley, C. ,
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7 h \ F 221 600°C and 1 atmosphere
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223 e I'
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R L ' -1 9mm O.D. 5mm I.D. 45mm 0.D
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Figure 5.- Paschen's law curves. 2-
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\ '? I The water-free product gases
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N I + 0" ON i I + 0 u / 0 0 I 0 cu
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- 233 SOME PROBLEMS OF THE KINETICS
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.. . :. ,. .I , . i ? .. . , ... .
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237 Table 2 Experimental Variables
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239 Zhbie I Eerccnt Consumption of
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241 Discussion The systematic varia
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I \ 1 243 FORMATION OF HYDROCARBONS
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h z - a o m a 20 T IME, minutes . F
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I 1 I I I I 0 I 2 3 4 5 TIME, minut
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The next five coluws in table 1 sho
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\ .\ t 251 Given the existence of t
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I L 253 Epple, R. P. and C. M. Apt.
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1 ' Fig. 1 Schematic of flow discha
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5' . ' I 1 257 co, with excess H2,
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1 1 1 moo 1400 1300 c V' I IPOO I I
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i 25i The Dlssocfatior of ToIuere V
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L ! , c PRODUCTS FROM A 28 MC. DISC
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'\ J ?. , .. . : PRODUCT FORMATION
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'9 / I '\ "1 BENZYL CATION AND RADI
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a
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271 tube serve? as the high voltare
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273 ion (1L.). Zxcitei-ion by colli
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Apparatus and Procedure 275 EXPERIM
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. 277 6. A freshly prepared sam le
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observed. The polystyrene (10% solu
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i i (12) c (11) (14) I 281 LITERATU
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FLOW- METER I ADDITIVE SUPPLY * ,28
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285 TABLE 2 Effect of Haloqenated A
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ANALYTICAL RESULTS Some evidence wa
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DISCUSSION 289 The salient features
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? ~ MENBERSHIP IN THE DIVISION OF F
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292 flow of the reactant gas stream
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294 have suitable residence times i
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0 E < h( E l! d K c 0 .- Y 0 t u t
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298 yields of many chemical product
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- ;i Y . 15. Pressure lOmm 5 > 10-
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302 the best and in many practical
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GENERATION AND MEASUREMENT OF AUDIO
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. The transformer secondary and the
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Vaccum-Tube Amplifier The mobile co
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310 f = Power supply frequency in c
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FUFARCI! INSTITUTE OF TFYDLC UNIVER
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J # I / 4) I . . '8 r4 0 r( P
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317 i Cuencb svsten w.nnar;itus use
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epcrte? the noss~kil.itv of nroduct
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1' b t +
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323 ....... - . . . . . . . . . . .
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1 \ i I i , / / / 8 3 1 325 To205 +
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- .- - - . - - . . . - . 327 n + c
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' POWER PLASMA GAS l e , ' I ! I I
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331 f'ENI?AL PF'FCLCCFC Dernis, P.R
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i J 333 ; mosphere (as opposed to a
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; it raised the question, still &?z
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p .I V I .= - - HCN/C(CALC. WITH C
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1 1 339 atmospheric ressure and ach
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RESULTS 341 Composition Dependence
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0.09 0.08 0.07 9 0.06 2 U - .$ 0.05
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II \ to the Slot So that less of th
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i 4 2 HYDROCARBON-NITROGEN REACTION
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I 1 349 c M m ; a e, k M x
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1.0 I - a. I n TEMPERATURE - OK Fig
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353 the experimental results in the
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,) 355 The ceaswed conversion cf ni
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1 6 357 Freezing. 3jpotnesise thzf
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359 \ Frozen Compositior: Calcillat
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I 1 \ 361 -. ne reaction proceecis
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\ 36 3 ' h, I 26. H. Purnell, Gas C
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In experiments on the direct conver
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367 used as blnders, with different
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369 ' i 1. REFERENCES Berber, John
Page 372 and 373: Distribution and yield rates of pro
Page 374 and 375: . . I . I 370 . . . . ., . . .. . .
Page 376 and 377: 4 372 090- > E w - m c N O - 0 z :
Page 378 and 379: A-Feed tank 6-Thermocracker GReceiv
Page 380 and 381: 80 \ 0 70 60 e 40 a U VI 9 30 20 10
Page 382 and 383: COAL DEASH& AND HIGH-PURITY COKE Wa
Page 384 and 385: 3Pn _. -. - L -J:,J.-;~~~L, ):as se
Page 386 and 387: S ~ l ~ o n~pg:ading r is the resul
Page 388 and 389: The range ~f temperatures and gener
Page 390 and 391: . .. 386 9 * - r. Y 2 .' d a f' r.
Page 392 and 393: .) .L m 388 I
Page 394 and 395: TABLE 4 390 DELAYED COKING OF DEASH
Page 396 and 397: , ! I- on '---
Page 398 and 399: 394 The present method is to keep t
Page 400 and 401: 396 ‘c erperature, while the pres
Page 402 and 403: 2, '! ! Proximate Analysis, wt $ Mo
Page 404 and 405: 0 IS 0 14 LL 9 013 e \ 3 b- m *- 01
Page 406 and 407: 402 HYDROGEN CYANIDE PRODUCED FROM
Page 408 and 409: 404 Before startup, the system is p
Page 410 and 411: 4 OL. ' , I. . TesCs. With.Coals .o
Page 412 and 413: Table 3.- Product Gas Analyses and
Page 414 and 415: 410 BIBLIOGRAPHY 1. American Public
Page 416 and 417: Figure 2. Enclosure surrounding hyd
Page 418 and 419: 0 0 f v) C 0 u m I z 2 c 2 r d J w
Page 420 and 421: 0. E c .4 7 .. .c . I ( - Low tempe
Page 424 and 425: 420 Ir ?Y ? ? 9 9 9 pc rod n o c o
Page 426 and 427: 422 Table 3. Room-texperature M'dss
Page 428 and 429: 424 state, depending on the strengt
Page 430 and 431: Table 4. Room-?;ergerature isomer s
Page 432 and 433: I' 1.3 . /o 9 IO 9 6 a 425 F F 33 I
Page 434 and 435: Brooks J.D. and Sternhell S. (1957)
Page 436 and 437: (52) Gib3 T.C. and Greenwood N.N. (
Page 438 and 439: 434 transducer vas then introduced
Page 440 and 441: 436 yield is quite similar. The con
Page 442 and 443: ?-!??? 0 mv, Uh\OhIe . . . . eirlrl
Page 444 and 445: 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 4
Page 446 and 447: 442 CHEMICAL REACTIONS IN A CORONA
Page 448 and 449: helium 444 CORONA REACTOR SYSTEM Fi
Page 450 and 451: 446 The ultraviolet spectrum. for t
Page 452 and 453: Biphenyl Fraction 448 The low molec
Page 454 and 455: LUd The actual structural definitio
Page 456 and 457: I I I I I In m 9 In 2 , I: r- In m
Page 458 and 459: ’. 454 Mechanism I The available
Page 460 and 461: 456 , , . The relatively low yield
Page 462 and 463: 458 h/lethylacetylene, allene and b
Page 464 and 465: Introduction VAPOR PHASE DECOMPOSIT
Page 466 and 467: 462 more efficient hydrogenation. T
Page 468 and 469: 464 place in parallel with fragment
Page 470 and 471: 466 P rl 0, k 7 rnI rn al k a I hl
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458 TABLE I. COMPOSI'IION OF GASEOU
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REFERENCES 1. C. Hirayama and D. A.
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i 472 Reciprocal Arc Enthalpy ,-> F
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474 be pumped down without altering
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476 Instead a hydrogen deficient fi
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i 478
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480 FATTY ACIDS AND n-ALKANES IN GR
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482 TA5L,E 2. - Carbon number distr
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6. 7. a. 9. 484 Lawlor, D. L., and
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' I ' Sample No. 6 ' 12 IO 8 6 z 4
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. 488 uiolecular weight of which ca
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Xississippi (Sample GS). Stock solu
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492 found at 5.7 and 4.9& for the W
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494 mechanisms. However, the voltad
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For pure polynuclcar arom.i;ic hydr
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- '-'. . ' . . values are listed in
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500 (1;) Ten, T. 17.: a;1d,Dic;
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- ~ Resistivity Czlculation 2: 1 j:
Page 508 and 509:
504 o ' C 0s 2 0 v x i 8 2 0 ! P -
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506 i
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d 601 L P LL
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I I I I I I I I m W N W N 0 (D ? 0
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514 was heated under nitrogen in a
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The line broadening at 79OK of the
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13. 14. 15. 16. 17. 18. 19. 20. 21.
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W L, Z 6 m (1: 0 6 d j o 2 ' 1 0.0
Page 526 and 527:
Coals 522 Studies of the 1600 cm-l
Page 528 and 529:
L in ole i c a c id - 0' Two sample
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526 Table 1.- Ultimate analyses of
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528 6. Friedel, R. A., and H. Retco
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egeneration. The system can be seen
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532 and can be expressed in terms o
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534 in the vapor increases with inc
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NH3 NH3 NH3 NH3 Pyridine Pyridine P
Page 542 and 543:
Mole Ratio of Test No. Quinoline to
Page 544 and 545:
IXPROFJCTION D; M. Mason Institute
Page 546 and 547:
-4:c~rciiny to recent studies o ;i4
Page 548 and 549:
544 Table 1. LIGHT EMISSION OF Y"TR
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emission in a few cases may be by d
Page 552 and 553:
LITERATUR2 CITED i. C. -. .' * il.
Page 554 and 555:
co, CH,,OR 1 - OTHER ADDITIVE FRITT
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FRIT 'TED CO, CH,.OR 4 ___ OTHER AD
Page 558 and 559:
340 350 300 400 4 50 500 600 700 80
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0 554 WITH COOLING (PLATE AT 40°C)
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5 56 then t = to when e = 0 2) the
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5 58 The surface heat transfer coef
Page 566 and 567:
Discussion and Results 560 Three br
Page 568 and 569:
__- ._ 562 Table I THERMAL AND PHYS
Page 570:
ln 4 I 0 4J v \ 1.0 0.8 0.6 L - 0.4
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