Practice of Kinetics (Comprehensive Chemical Kinetics, Volume 1)

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4 ANALYSIS 85when hydrogen is used2". The detector block has to be thermostatted very accurately.The sensitivity of the detector is as good or better than the katharometer.4.3.6 Product identijication and trappingAn initial product identification can be carried out by comparing the retentiontimes, under given conditions, of the unknown compound with that of suspectedknown compounds. To couhteract minor variations in flow rate and temperature,coincidence of peaks can be checked with consecutive doping or marking of themixture with known compounds. Coincidence should also be checked by usingone or more different columns. In this context the gas density balance detectorprovides particular confidence in identification.Conclusive evidence is produced by infrared or mass spectroscopic methods. Thisinvolves the selective trapping of each product as it is eluted from the column.Efficient trapping is obtained by quenching in two or more U-tubes containingglass wool followed by trapping in a breakseal trap for subsequent analysis (Fig.56). Flow may be diverted to this trapping system by a 3-way solenoid valve operatedby a micro-switch. The latter is activated by the pen of the recorder incorporatedin the GLC when the peak due to the required material reaches 80 % of its maximum.This system has also been used on a small preparative scale.Micro -switchGL.XiFtube"Araldite" jointsGlass-wok packed trapsFig. 56. Product trapping from a OLC exit tube.4.3.7 Sampling and quantitative estimationSamples may be taken for analysis at once, or after fractionation of the productsand reactants. A set-up due to Porter and Norrish"', is shown in Fig. 57. A sampleReferences pp. 104-1 11
86 EXPERIMENTAL METHODS FOR SLOW REACTIONSFig. 57. Multi-column technique for product analysis. From ref. 280.3,4 Sample volumeAll ports are isolated exceptthose connecting carrier gassupply to cdumnDivision of valve actionby arrangement of portsInjection of sampleEvacuation of sample volumeFilling of sample volume fromfrom reaction vesselFig. 58. Gas-sampling valve. From ref. 282.
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COMPREHENSIVE CHEMICAL KINETICS
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P.O.ELSEVIER PUBLISHING COMPANY335
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Contributors to Volume 1L. BATTDepa
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XCONTENTS4.3 Gas chromatography ...
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XI1CONTENTS4.6 Magnetic measurement
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4 EXPERIMENTAL METHODS FOR SLOW REA
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Reaction Furnace CircuitI10 EXPERIM
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178 REFERENCES46 M. EIGEN AND L. DE
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Chapter 3Experimental Methods for t
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182 EXPERIMENTAL METHODS FOR HETERO
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192 EXPERIMENT A L MET H 0 D S F 0
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194 EXPERIMENT A L MET H o D s F o
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206 EXPERXMENTAL METHODS FOR HETERO
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222 EXPERIMENT A L METHODS F 0 R HE
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230 EXPERIMENT A L METHOD s FOR HET
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236 EXPERIMENT A L METHOD s FOR HE
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242 EXPERIMENT A L ME TH 0 D S FOR
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248 EXPERIMENT A L METHOD s F o R H
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254 EXPERIMENTAL MET HODS FOR HETER
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258 EXPERIMENT A L METHODS F 0 R HE
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266 EXPERIMENT A L MET H o D s F o
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270 EXPERIMENTAL MET HODS FOR HE TE
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274 EXPERIMENT A L METHOD s FOR HE
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280 DETECTION AND ESTIMATION OF INT
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344 TREATMENT OF EXPERIMENTAL DATAf
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346 TREATMENT OF EXPERIMENTAL DATAp
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348 TREATMENT OF EXPERIMENTAL DATAg
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IndexAabsorption cross section, che
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424 INDEXbenzyl chloride, matrix ph
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426 INDEXchlorine (contdj—, react
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428 INDEXdeuterium oxide, addition
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430 INDEXentropy change, in radical
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432 INDEXfrequency of oscillation,
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434 INDEXhydrogen atoms (contdj—,
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436 INDEXisotopes (contd.J—, use
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438 INDEXmethyl radicals, chain ter
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440 INDEXoctadiene, ESR determinati
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442 INDEXphotoelectric measurement,
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444 INDEXrad, definition of, 66radi
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446 INDEXSchmidt number, and mass t
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448 INDEXTtailing reducer, in gas c
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450 INDEXviscosity, and diffusion c
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Practice of Kinetics (Comprehensive Chemical Kinetics, Volume 1)

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