On the unexpected behavior of a common gas chromatographic phase

Aue, Walter A.; Hastings, Corazon R.; Kapila, Shubhender

doi:10.1016/s0021-9673(00)92196-4

Cited by 187 publications

(27 citation statements)

References 12 publications

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“…These results are similar to those obtained by Aue et al 1 who used temperature treatments of 260 ºC to 280 ºC for 12 h. In that work the chromatographic behavior of polar compounds showed symmetric peaks with very short retention times. This result is confirmed by thermogravimetric simulation where we observe that the immobilized packing lost 3.5 % of the stationary phase while the non-immobilized packing lost 11.0 % of stationary phase at 300 °C.…”

Section: Discussionsupporting

confidence: 91%

“…Immobilization of the stationary phase is generally achieved by bonding the polymer chain to the support. This immobilization process is initiated by free radicals which are produced by heat [1][2][3][4][5] , chemical initiators such as azocompounds [6][7][8] , peroxides [9][10][11][12][13] or ozone 14,15 , and ionizing radiation such as electrons 16 , gamma radiation 17,18 and low-temperature plasmas 19 . All these methods have been successfully applied to produce immobilized nonpolar silicone phases within capillary columns.…”

Section: Introductionmentioning

confidence: 99%

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Preparation of thermostable poly(ethylene glycol) using thermal treatment in sealed system

Cardoso¹,

Copetti²,

Schwerz³

et al. 2000

J. Braz. Chem. Soc.

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O trabalho descreve um método rápido para a preparação de Carbowax 20M imobilizada sobre suporte, através do uso de tratamento térmico em forno convencional. O processo de extração com solventes remove a fase estacionária não imobilizada de poli(etileno glicol) (PEG) do suporte e a diferença de massa antes e após a extração fornece o percentual extraído e, consequentemente, o percentual total imobilizado. O tratamento térmico a 250 °C por 10 horas mostrou que a imobilização reduziu a atividade do material e aumentou o número de pratos (N) e a resolução (Rs), enquanto o fator de retenção (k) reduziu. Desta forma, a separação na coluna com material tratado é mais rápida e mais eficiente. A rapid method is described for preparation of support -bonded Carbowax 20M columns packing using a conventional furnace to heat the packing. Solvent extraction of the stationary phase removes the non-immobilized poly(ethylene glycol) (PEG) from the support and the difference between final and initial weight provides the total percent extracted and, consequently, the total percent immobilized. Treatment of the packing material at 250 °C for 10 h. reveals that the immobilization reduces the material activity and increases the plates number (N) and resolution (Rs) while the retention factor (k) is decreased. Thus, separations with this treated column are faster and display higher efficiency.

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Section: Discussionsupporting

confidence: 91%

Section: Introductionmentioning

confidence: 99%

Preparation of thermostable poly(ethylene glycol) using thermal treatment in sealed system

Cardoso¹,

Copetti²,

Schwerz³

et al. 2000

J. Braz. Chem. Soc.

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“…Mepl ions were removed from column 1 by filling the capillary with 20% HCI solution, sealing the ends and heating at 180°C for 14 h. After rinsing with 0.5 M HCI, a barium carbonate layerwas deposited on the interior wall by pushing a saturated solution of barium hydroxide through the column with carbon dioxide gas [14,15]. The column was deactivated with a nonextractable layer of Carbowax 20 M by a method similar to that of Aue et al [16]. A 0.5Y0 (w/v) solution of Carbowax 20 M in chloroform, followed by a 5 cm mercury plug was pushed through the column at a rate of approximately 0.6 cmls by nitrogen.…”

Section: Gas Chromatographymentioning

confidence: 99%

High resolution glass capillary columns for the gas chromatographic analysis of alditol acetates of neutral and amino sugars

Hudson

Morgan

Fox

1982

J. High Resol. Chromatogr.

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SummaryThe development of improved high resolution glass capillary columns for separating the alditol acetates of neutral and amino sugars is described. Different capillary column treatments were evaluated for their activity toward amino sugar derivatives and for their effect on the efficiency of the completed column. The simple two-step procedure of leaching with aqueous hydrochloric acid and dynamic coating with SP-2330 was found to produce efficient and inert columns.

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“…These prob lems are ame lio rated by the im mo bi li za tion of the sta tion ary phase through bond ing be tween the polymer chains with pos si ble bond ing to the sup port. This immo bi li za tion pro cess is ini ti ated by free rad i cals which are pro duced by heat [1][2][3][4][5] , chem i cal ini ti a tors such as azocompounds [6][7][8] , per ox ides [9][10][11][12][13] or ozone 14,15 , and ion iz ing ra di a tion such as elec trons 16 , γ ra di a tion 17,18 , and low-temperature plas mas 19 . All of these meth ods have been suc cess fully ap plied to pro duce im mo bi lized nonpolar sil i cone phases within cap il lary col umns.…”

Section: Introductionmentioning

confidence: 99%

Peroxide immobilization of a silicone stationary phase on a support

Schneider¹,

Pizzutti²,

Adaime³

1997

J. Braz. Chem. Soc.

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A imobilização de uma fase estacionária de sil i cone (SE-30) sobre Chromosorb W-AW para uso em cromatografia gasosa foi iniciada por peróxido de dicumila (DCUP). Foram estudadas concentrações apropriadas de peróxido e o procedimento utilizado para imobilização é bem descrito.Foram realizados tes tes de extrações com solventes, avaliação cromatográfica, bem como estabilidade térmica e lavagem com solventes em coluna. Estes tes tes mostraram que a preparação de SE-30 imobilizada sobre Chromosorb W-AW, usando DCUP, é simples e produz fases estacionárias eficientes e resistentes a solventes.The im mo bi li za tion of a sil i cone sta tion ary phase (SE-30) on Chromosorb W/AW for use in packed col umn gas chro ma tog ra phy was ini ti ated by dicumyl per ox ide (DCUP). Ap pro priate per ox ide con cen tra tions were stud ied and the im mo bi li za tion pro ce dure is de scribe d.Sol vent ex trac tions and chro mato graphic test ing, as well as ther mal sta bil ity and on-column sol vent rins ing, showed that prep a ra tion of an SE-30 phase im mo bi lized on Chromosorb W/AW us ing DCUP is a sim ple method that pro duces ef fi cient and non-extractable sta tion ary phases. Key words: gas chro ma tog ra phy, packed col umns, or ganic per ox ide im mo bi li za tion, immo bi lized sta tion ary phases

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On the unexpected behavior of a common gas chromatographic phase

Cited by 187 publications

References 12 publications

Preparation of thermostable poly(ethylene glycol) using thermal treatment in sealed system

Preparation of thermostable poly(ethylene glycol) using thermal treatment in sealed system

High resolution glass capillary columns for the gas chromatographic analysis of alditol acetates of neutral and amino sugars

Peroxide immobilization of a silicone stationary phase on a support

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