On-column injection onto capillary columns. Part 2: Study of sampling conditions; practical recommendations

During one year continuous use of on-column injection, the typical advantages described in our first report have fully been confirmed. In addition the analysis of large sample volumes has proved promising. Only minor modifications have been applied to the on-column injector device. Broad evidence has been gathered showing that full separation efficiency of the capillary columns after on-column injection is attained only when cold trapping or the solvent effect, as band shortening mechanisms, are working- While, under the conditions of on-column injection, cold trapping is less efficient than with other injection techniques, the opposite holds true for the solvent effect. Compared with splitless injection, the danger of excessive solvent condensation on the column is increased. A working rule is presented for establishing the optimal chromatographic conditions for handling large sample volumes while ensuring full separation efficiency yet avoiding harm to the column.     

Gas-chromatographische Bestimmung von Mono-, Di- und Tri?thylenglykol in Wasser

Ohne Zusammenfassung

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Gas-chromatographie determination of ethylene glycol, diethylene glycol and triethylene glycol in water

     

Gas chromatography of halogens

Summary The semi-empirical theory on the retention volume in gas chromatography recently developed by some experiments, was found to require partial correction. It was newly refined and summarized. Overall experimental checking was performed by the use of Cl₂, Br₂, and I₂.

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Gas-Chromatographie von Halogenen

Zusammenfassung Die halbempirische Theorie über das Retentionsvolumen in der Gas-Chromatographie, die kürzlich an Hand einiger Versuche entwickelt wurde, erforderte eine teilweise Korrektur. Sie wurde verbessert und zusammenfassend dargestellt. Kontrollversuche wurden mit Hilfe von Chlor, Brom und Jod durchgeführt.

     

Preparation of apolar glass capillary columns by the barium carbonate procedure

As an extension of previous reports, the barium carbonate procedure has been optimized in detail for the preparation of apolar columns. The aim was to produce optimum overall column characteristics, and to maintain them unchanged under the prolonged influence of the highest possible temperature. The main parameters under optimization were glass variety, leaching of glass surface with aqueous HCl, and amount of barium carbonate deposited, while deactivation and coating were kept constant. The basic column characteristics were adsorption properties and thermostability of deactivation, acid/base behaviour and separation efficiency. They were determined by a new, quantitative testing procedure. Intense leaching was able to eliminate almost totally the differences between glass varieties and to create a well-defined glass surface. While untreated glass, leached glass, and barium carbonate treated glass showed specific weak points in the respective column quality, the combination of leaching and barium carbonate treatment yielded the highest and most stable quality. Some technical modifications of the preparation procedure are described, including deactivation in the gas phase, and use of pentane as a solvent for static coating.     

Application of a micro carbon rod atomizer as Br-spezific gas-chromatographic detector

Summary A micro carbon rod atomizer has been employed for specific and quantitative bromine determinations. This Br-specific gas-chromatographic detector works by help of InBr-bands and measurement at 372.7 nm. The performance of this flame band emission detector (FBD) is demonstrated by calibration curves and the detection limits of 2 examples (ethyl bromide, ethylene dibromide), the latter being 5 and 36 ng of bromine, respectively. The reproducibility has been found to be 4.3%. An example of this detector in comparison with a thermoconductivity detector (TCD) is presented.

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Verwendung einer Mikro-Graphitküvette als Br-spezifischer Detektor für die Gas-Chromatographie

Zusammenfassung Eine Mikro-Graphit-Küvette wird für spezifische quantitative Brombestimmungen nach der Indium-Methode bei 372,7 nm benützt und in Verbindung mit einem Gas-Chromatographen als Br-spezifischer Detektor eingesetzt. Die Leistungsfähigkeit dieses Detektors wird an 2 Beispielen (Äthylbromid, Dibromäthan) mit Hilfe von Eichkurven, Bestimmung von Nachweisgrenzen u. ä. demonstriert. Die Nachweisgrenzen liegen bei 5 bzw. 36 ng Brom für die 2 genannten Substanzen. Die Reproduzierbarkeit der Messungen liegt bei 4,3%. Ein Beispiel für die Registrierung eines Gemisches verschiedener Substanzen, gemessen mit dem GC + Flammen-Banden-emissions-Detektor (FBD) und zum Vergleich mit einem Wärmeleitfähigkeitsdetektor (TCD), wird dargestellt.

This research work was supported by financial help of the Bundesminister für Forschung und Technologie in Bonn (GFR).     

Gas chromatographic analysis of bifunctional amines after derivatization with methyldichlorophosphine and sulfur

Summary A derivatization procedure for the gas chromatographic analysis of bifunctional amines likeβ-adrenergic blocking drugs is described. The method consists of a two-step reaction with methyldichlorophosphine and sulfur in presence of triethylamine to form cyclic methylphosphonothioic derivatives. The properties of these compounds are discussed and the application of the method to the quantitation of ephedrine in human body fluids is presented. Presented at the 15th International Symposium on Chromatography, Nürnberg, October 1984     

氮气中电晕放电高能电子密度沿反应器分布的光谱研究

利用目前在等离子体特性诊断方面较为先进实用的发射光谱法,在常温常压下测量了正脉冲电晕放电Ｎ２（Ｃ３Πｕ→Ｂ３Πｇ）发射光谱相对强度沿线－筒式反应器的径向分布以及Ｏ２对Ｎ２（Ｃ３Πｕ→Ｂ３Πｇ）发射光谱强度的影响．由此得到了正脉冲电晕放电等离子体中高能电子（≥１１．０３ｅＶ）的电子密度沿线－筒式反应器的径向分布情况．     

Isolation of essential oils from tobacco by gas co-distillation/solvent extraction

Summary The essential oils have been isolated from tobacco leaves using a simple gas co-distillation apparatus. The method involves co-distillation with water under the continuous stream of an inert gas with subsequent single solvent extraction of the distillate. The extract is analysed on GC and GC/MS in splitless injection mode without further concentration. The method was evaluated for reproducibility using n-octadecane as an internal standard. The distillation-extraction procedure was reporducible with an average deviation of ±3% for the major constituents. The present method was applied to the analyses of the essential oils of other agricultural products.Dedicated to Dr. L. S. Ettre on the occasion of his 60th birthday.