Large scale preparative gel permeation chromatography

Montague, P. G.; Peaker, F. W.

doi:10.1002/polc.5070430124

J. polym. sci., C Polym. symp.

1973

DOI: 10.1002/polc.5070430124

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Large scale preparative gel permeation chromatography

P. G. Montague

F. W. Peaker

Abstract: The design and construction of a large‐scale gel permeation chromatographic unit is described, and it is a tenfold scale‐up of the usual analytical instrument. Important aspects of the column packing procedure are given. Fractions prepared using this apparatus were isolated and reinjected into an analytical instrument. In this way the efficiency of preparative fractionation was investigated using several polystyrene samples covering a wide range of molecular weights and distributions. Generally the highest mol… Show more

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1977

1983

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Cited by 8 publications

References 7 publications

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Beiträge zur gelchromatographischen Fraktionierung im präparativen Maßstab. Trennungen an kaskadenartigen Gelkombinationen

Albrecht

Glöckner

1980

Acta Polymerica

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Permanent-porose Polystyrole wurden als Tragcr hei priiparativ-gelchromatographischen Fraktionierungen eingesetzt, wobei sowohl uber die Testung einzelner Gcltypen als auch ihrer Kombinationen berichtet wird. Fur Gelkombinationen, bei denen die Trager entsprechend abnehmender mittlerer PorengroDe angeordnet waren, ergab sicli trotz geeigneter Einzeltriger keine ausreichende Trennfiihigkeit uber den gcsamten Molmassenbereich. Die Crsache fur dieses Verhalten wird experimentell aufgezeigt. Hccnei?osaw.m no @parcyuonuposaHum &emodo& npenapamusfiotl zem-xpowamozpa$uu. I . npoqeccbi pa3dene~u.u c ucno~zb30ea~lue.~ cnoes zenetl e sude rcacxaaosPermanently porous polystyrenes were used as carriers in preparative gelchromatographic fractionation experiments. The testing of various kinds of gels and their combination is described. With gel combinations, the carriers of which were arranged with respect to decreasing average pore size, no sufficient separation on the entire molecular range was achieved despite the use of appropriate carriers. The cause of this behaviour is explaincd by experimental results.

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Beiträge zur gelchromatographischen Fraktionierung im präparativen Maßstab. Trennungen an kaskadenartigen Gelkombinationen

Albrecht

Glöckner

1980

Acta Polymerica

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Beiträge zur gelchromatographischen Fraktionierung im präparativen Maßstab. II. Zum Einfluß der Gelanordnung auf das Elutionsverhalten und die Trennqualität

Albrecht

Glöckner

1980

Acta Polymerica

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Ausgehend von einer Analyse des Einflusses der Gelanorduung auf die Trennqualitat bei praparativ-gelchromattrgraphischen Fraktionierungen werden Ergebnisse zum Elutionsverhalten und zur Differenzierfahigkeit bei unterschiedlicheu Gelanordnungen mitgeteilt,. Die Iintersuchung zeigte, dalJ bei der praparativen GPC neben geeigneten Tragern die Gelanordnung entscheidend die erreichbare Trenneffektivitat und damit den erforderlichen Fraktionieraufwand beeinflufit. Die Ursache hierfiir ist in koiizentratiolishedingten Veriinderungen des gelchromatographisrh~~n Trennprozesses zu sehen. MccJtedosafiua no $pa?cyuonuposanuroAerno8oa npenapamusnoii aenb-xpowamozpa$uu. I I . 0 sJtumuu pacnonoxcetmfi cmes rta nosedeMue n p u a~ttouposanuu u a$$ie~rnu~nocrnb pa313enenuz L~X O~F I 113 aaanma BJIHFIHAFI pacnonoxeHm emoeB Ha ~@ @~K T H B H O C T~ pasneneam n p~ @paKiinompoBamm a Tamie 06 ~@ @~K T H B H O C T H p a 3~e n e~m B cnyqae P~B J I A~H~I X paenonowemti renefi B C~O F I X . klccne~osawm noKa3am11, w o ~aprxny c npmronHocTbm Hocarenei paenonoweme renei B CJIOFIX peuramqm 06pa30M onpe,qenxeT IIpmmiaM~ 3~0 r o RRJIFIIOTCFI ~~B H C F I~P I~ OT RoHqewrpatim nmeifemfi R npouecce renb-xpoMaTorpa~nserKoro p a 3~e n e~m~.Contributions to the gel ckrornatograph ic fraAonation on preparative scale. I I . The effect of gel arrangetneni on the elfttion behaviour and the separation quality Rased on the determination of the effect of gel arrangement on the separation quality in preparative gelchromatographic separation the results on the elution behaviour and differentiation ability of different gel arrangements are described. Besides suitable carriers the gel arrangement was found to affect decisively the separation activity and thus the efficiency of fractionation. This is obviously caused hy concentration-dependent changes of the gelchromatographic scparation proct'ss.MeTOAOM IIpeIIapaTEBHOfi rnx IIPHBORFITCFI 3KCrIePLIMeIITaJIbMLie HaHHbIe 0 IIOBeReH1111 re.TIefi npll 3JIIO11pORaHHI<, XOCTPIFaeMJ'H, 3@@eKTKBAOCTb pa3AeJIeH1153 11 TeM CaMLIM HeO6XOARMYlO TPj'~OeMEOCTL npG1 @paKI~~~H11pORaH1111.

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Preparative gel permeation chromatography. I. Polypropylene

Vaughan¹,

Francis²

1977

J of Applied Polymer Sci

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SynopsisPreparative gel permeation chromatography was used to produce a number of polypropylene reference samples, within the molecular weight range of 10,000-600,OoO, from commercial materials. Some of these materials were degraded in a controlled manner to give base materials having suitable molecular weight characteristics. A procedure has been developed using a single preparative column packed with equal quantities of Styragel with nominal exclusion limits of lo2, lo3, lo4, and lo5 nm.The volume of solvent for recovery was minimized by use of higher loading factors than in analytical GPC (some 2-20 times more polymer was thus fractionated in each experiment). Under these conditions the fractions first eluted were sharpest having polydispersities of about 1.5. First fractions, from different base materials, were characterized by analytical GPC, and those of similar molecular weight and polydispersity were combined to give the reference samples. Refractionation was necessary with the highest molecular weight base material because the first stage fractions were not sharp enough. Some of these fractions were recovered at elution volumes where much lower molecular weight material was expected. Comparison with results from the other base materials indicates that the primary cause of the spreading is not overloading. This spreading is explained in terms of slower partitioning of the larger molecules between the interstitial fluid and the gel particles.

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Large scale preparative gel permeation chromatography

Cited by 8 publications

References 7 publications

Beiträge zur gelchromatographischen Fraktionierung im präparativen Maßstab. Trennungen an kaskadenartigen Gelkombinationen

Beiträge zur gelchromatographischen Fraktionierung im präparativen Maßstab. Trennungen an kaskadenartigen Gelkombinationen

Beiträge zur gelchromatographischen Fraktionierung im präparativen Maßstab. II. Zum Einfluß der Gelanordnung auf das Elutionsverhalten und die Trennqualität

Preparative gel permeation chromatography. I. Polypropylene

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