chemical physics of discharges - Argonne National Laboratory
chemical physics of discharges - Argonne National Laboratory chemical physics of discharges - Argonne National Laboratory
Xississippi (Sample GS). Stock solutions in benzene of iodine and of the individual asphaltenes were made up in fixed concentration and samples I of varied composition prepared by mixing appropriate quantities of these stock solutions at room temperature and lyophylizing at reduced pressure to yield powdered solids with a homogeneous iodine distribution. These samTles were analyzed before and after the electrical measurements for $1 by ignition in oxygen, reduction with hydrazine sulfate, and poteniometric , titration of the resulting iodide with &NO3 using a Beckman model K automatic titrator. Usually there was no observable loss of free iodine during electrical measurements; lO-l5$ loss of iodine was found after degassing. The iodine values used in the present work are those values obtained after completion of the electrical measurements for the entire specimen. Treatment of Data The resistance values along with the corresponding temperature data and dimensions of the specimen were key punched on IEiM cards and evaluated on an IBM 7090-1401 digital computer system. Given A, the area of the cross section, and L, the Length of the specimen, the resistivity, p, can be evaluated from the resistance, R, as follows: p = AR/L. The temperature dependence of the resistivity is then evaluated by the relationship: 4 PT = 00 exp (+kT), i where k is Boltzman's constant, E is the energy gap in eV and po is the resistivity extrapolated to ,$ = 0. By use of a California Computer Products % 30-in. plotter (300 steps; l/5OO-in. per step) the temperature dependence data were fitted to straight lines (Fig. 2) as given by the equation \ < \ \. V \ 4
3' I / 3 2 b V t 491 log p = log pJ-€E/(2kT In 10) From the digital output, p250c and E can be obtained. The applied voltage I was limited to values under LO V; in this region Ohm's law was followed. The temperature range examined was from ambient to 90°C. There is error involved in any single measurement of resistance, owing to systematic errors in the electrometer; errors also enter in the measurement of the dimensions of the specimen. That the results were not influenced by such systematic errors is evident from the two sets of data for two different preparations of an asphaltene (VY)-iodine complex, as given in Table I. The uncertainties in the per cent iodine and sample size may be judged from the variations in the independent measurements. Despite these variations, the resistivity at 2 5 O C and the energy gap are within ca. 5% of the mean values. Infrared Analysis Differential IR spectra were obtained from a scan of an iodine- containing asphaltene versus a reference asphaltene at equal asphaltene concentration in CSg (the iodine-containing sample is normalized to lo@$ asphaltene for purposes of comparison) using a Beckman IR-12 instrument. A control scan of asphaltene in CS2 solution against itself also was made for each sample. X-ray Diffraction A Norelco x-ray diffractometer equipped with a CuxGL radiation source and a geiger tube detector was used to study the asphaltene-iodine system. In order to record the shift of the d-spacing due only to change in mass absorption coefficients, adamantane was added to an asphaltene- iodine complex (24% I) and to the original asphaltene. Strong (111) and (260) reflections due to the adamantane mixed with the VY asphaltene were
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- Page 446 and 447: 442 CHEMICAL REACTIONS IN A CORONA
- Page 448 and 449: helium 444 CORONA REACTOR SYSTEM Fi
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- 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
- Page 472 and 473: 458 TABLE I. COMPOSI'IION OF GASEOU
- Page 474 and 475: REFERENCES 1. C. Hirayama and D. A.
- Page 476 and 477: i 472 Reciprocal Arc Enthalpy ,-> F
- Page 478 and 479: 474 be pumped down without altering
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- Page 482 and 483: i 478
- Page 484 and 485: 480 FATTY ACIDS AND n-ALKANES IN GR
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- Page 488 and 489: 6. 7. a. 9. 484 Lawlor, D. L., and
- Page 490 and 491: ' I ' Sample No. 6 ' 12 IO 8 6 z 4
- Page 492 and 493: . 488 uiolecular weight of which ca
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3'<br />
I<br />
/<br />
3<br />
2 b<br />
V<br />
t<br />
491<br />
log p = log pJ-€E/(2kT In 10)<br />
From the digital output, p250c and E can be obtained. The applied voltage<br />
I<br />
was limited to values under LO V; in this region Ohm's law was followed.<br />
The temperature range examined was from ambient to 90°C.<br />
There is error involved in any single measurement <strong>of</strong> resistance,<br />
owing to systematic errors in the electrometer; errors also enter in the<br />
measurement <strong>of</strong> the dimensions <strong>of</strong> the specimen. That the results were not<br />
influenced by such systematic errors is evident from the two sets <strong>of</strong> data<br />
for two different preparations <strong>of</strong> an asphaltene (VY)-iodine complex, as<br />
given in Table I. The uncertainties in the per cent iodine and sample<br />
size may be judged from the variations in the independent measurements.<br />
Despite these variations, the resistivity at 2 5 O C and the energy gap are<br />
within ca. 5% <strong>of</strong> the mean values.<br />
Infrared Analysis<br />
Differential IR spectra were obtained from a scan <strong>of</strong> an iodine-<br />
containing asphaltene versus a reference asphaltene at equal asphaltene<br />
concentration in CSg (the iodine-containing sample is normalized to lo@$<br />
asphaltene for purposes <strong>of</strong> comparison) using a Beckman IR-12 instrument.<br />
A control scan <strong>of</strong> asphaltene in CS2 solution against itself also was made<br />
for each sample.<br />
X-ray Diffraction<br />
A Norelco x-ray diffractometer equipped with a CuxGL radiation<br />
source and a geiger tube detector was used to study the asphaltene-iodine<br />
system. In order to record the shift <strong>of</strong> the d-spacing due only to change<br />
in mass absorption coefficients, adamantane was added to an asphaltene-<br />
iodine complex (24% I) and to the original asphaltene.<br />
Strong (111) and<br />
(260) reflections due to the adamantane mixed with the VY asphaltene were