Pr�parative Gaschromatographie

Bayer, Ernst; Witsch, H. G.

doi:10.1007/bf00448578

Cited by 10 publications

(5 citation statements)

References 8 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…For preparative work a high ratio of liquid phase to solid support is desirable (8,12), but in the present study the degree of separation deteriorated when 20y0 or inore liquid phase was used. A ratio of 1 : 6 was found to give consistelltly good results.…”

Section: Initial Expe~inzentsmentioning

confidence: 63%

The Separation of Some Terpenoid Compounds by Gas–liquid Chromatography

Rudloff¹

1960

Can. J. Chem.

View full text Add to dashboard Cite

A study has been made of the degree of separation of mixtures of some terpene hydrocarbons, some of their oxygenated derivatives, two sesquiterpene alcohols, and three monophenols 011 a variety of colulnns. Temperature and sample size affected the degree of separation and the solid support Chromosorb \V, a calcined diatomaceous earth, was found to combine the advantages of Celite and C-22 firebrick without causing decomposition of the sample a t higher temperatures. When Craig polyesters were used as liquid phases, separations equal to those obtained on polyethylene glycol were realized with the added advantage that these produced columns which are stable a t 190 to 220' C. Consequently, sesquiterpene alcohols and ~~~o~~o p h e n o l s were also separated successfully. Another useful liquid phase for both low and high temperatures was found in a meta-linked polyphenyl ether. Squalene was found to be a n efficient liquid phase for the separation of terpene hydrocarbons a t 130' C and lower. The possible application of the present findings for preparative work is discussed. INTRODUCTIONA general method for the separation of small amounts of closely related terpene hydrocarbons, some of their oxygenated derivatives as well as some higher boiling sesquiterpene alcohols and monophenols, was required in this laboratory. Sucll mixtures often have a narrow range of boiling points and separation by fractional distillation not only requires large amounts, but frequently fails to produce pure components. Gas-liquid chrornatography (GLC) offers considerable advantages over fractional distillation when quantities of 0.01 to 0.1 g arc required, and has in several instances been extended to the gram scale. This technique was, therefore, studied in some detail to find suitable conditions for colnplete separation of such terpenoid mixtures 011 a 0.1-to 1-g scale. The experiments were can-iecl out with a Beckman GC-2 chro~natograph, using helium as carrier gas, a thermal conductivity cell as detector, and 6-foot columlls of 6-mm inner diameter.Successful separations of terpenoid co~npounds by GLC have been described in the literature. Bernhard (I) separated five monoterpene hydrocarbons on 20-foot polyethylene glycol and n-octyl phthalate columns, but obtained poor results when silicone fluid, Apiezon L , or high vacuunl grease was used as liquid phase. Bayer et al. (2) used hydrogen as carrier gas and obtained a fair degree of separation for a large variety of terpenoid compounds on columns containing silicone vacuum grease to which alkali capronates had been added. Cvrkal and Janhk (3), also using hydrogen, obtained good results for

show abstract

Section: Initial Expe~inzentsmentioning

confidence: 63%

The Separation of Some Terpenoid Compounds by Gas–liquid Chromatography

Rudloff¹

1960

Can. J. Chem.

View full text Add to dashboard Cite

show abstract

“…For these investigations different apparatus were used (1)(2)(3)(4)(5)(6)(7)(8)10). The columns varied between 0.4-cm.…”

Section: Apparatus and Methodsmentioning

confidence: 99%

“…The specifications (1,3,7,11,15) especially given for preparative columns are similar to alchemistic recipes, and are not reproducible because of lacking experimental data. Our investigations showed that rocking operations with only one dimension moving-i.e., vibration, pushing, or tappingis not satisfactory.…”

Section: Reproducibility Of Column Packingmentioning

confidence: 99%

“…An expansion of gas chromatography to separation of greater amounts of substances (1 to 1000 grams per separation cycle) may be realized primarily by increasing column diameter. Though upscaling of gas chromatography primarily was hampered by fundamental reflections (12), theoretical considerations (9), and experiments (5), the investigations of Bayer, et al (1)(2)(3)(4)(5)(6)(7)(8) and later Huyten, et al (11) made evident, that by careful column filling and appropriate apparatus the loss in efficiency is tolerable.…”

Section: Wall-effect In Packed Columnsmentioning

confidence: 99%

“…Golay's patent (3) on capillary columns includes a number of claims which pertain to capillary adsorption columns, but the specific directions for column preparation which are disclosed, and the illustrative chromatograms, refer to capillary partition columns. Likewise, during the past few years, the Perkin-Elmer Corp. has extensively advertised capillary partition columns and has published papers demonstrating their advantages, but it has never mentioned the preparation or the use of a capillary adsorption column.…”

Section: Columnsmentioning

confidence: 99%

See 2 more Smart Citations

Filling of Analytical and Preparative Columns for Gas Chromatography.

Bayer¹,

Hupe²,

Mack³

1963

Anal. Chem.

View full text Add to dashboard Cite

Präparative Gaschromatographie

1961

View full text Add to dashboard Cite

E r g a n z u n g e n bei d e r K o r r e k t u r :Nach Fertigstellung dieser Arbeit sind zwei wichtige Entwicklungen mitgeteilt worden. 7.7.8.8-Tetracyan-chinodimethan ( V ) wurde dargestellt; durch Aufnahme eines Elektrons bildet es leicht ein stabiles Anion-Radikal. Gewisse Salze dieses Anion-Radikals iibertreffen in ihrer II NC-C-CN V VI elektrischen Leitfahigkeit alle bis jetzt gemessenen organischen V e r b i n d~n g e n~~) . Wallenfels und B a e h w~a n n~~) haben Tetracyanchinon ( V I ) dargestellt. Dieses ist eine sehr starke n-Saure und ein derart starkes Oxydationsmittel, dall es raseh durch Alkohol, Tetralin und sogar Wasser zum Hydrochinon reduziert wird.

show abstract

Pr�parative Gaschromatographie

Cited by 10 publications

References 8 publications

The Separation of Some Terpenoid Compounds by Gas–liquid Chromatography

The Separation of Some Terpenoid Compounds by Gas–liquid Chromatography

Filling of Analytical and Preparative Columns for Gas Chromatography.

Präparative Gaschromatographie

Contact Info

Product

Resources

About