A new column-based preparative fractionation instrument, capable to fractionate up to 20 grams of polymer.
Fully Automated Column-based Preparative (PREP) Fractionation Equipment for Polymers.
PREP C20 is a fully-automated preparative pilot-plant-type equipment designed to fractionate, in a column’s support, high amounts of polymer according to its Chemical Composition by a Temperature Rising Elution Fractionation (TREF) process, or according to its Molar Mass, by modifying the solvent strength through a solvent-non solvent combination, typically in isothermal conditions.
A dry sample is put in a vessel and filled with solvent for dissolution. The sample solution is then loaded into a column where the crystallization takes place. The equipment fractionates the sample following the selected method’s conditions and the number of fractions, which can be eluted at the desired volumes. In the end, the vessel is rinsed and ready for the following fractionation.
The main steps in the preparative fractionation process (dissolution, column loading, crystallization, elution, and fraction collection) are performed in an automatic mode, thus, avoiding the need for handling hot and large amounts of solvent. It is precisely in its capacity of fully automating the fractionation of large amounts of polymer where the system holds its major benefit.
PREP C20 facilitates cross-fractionation studies (fractionation through TREF or Molar Mass and follow up analysis through GPC/SEC or TREF), that have been demonstrated to be a necessary tool to fully characterize resins. The fractions obtained can be further analyzed by spectroscopic techniques and can be used for micromechanical testing as well.
· Up to 20 grams of polymer, depending on the sample
· Column-based fractionation
· Unlimited number of fractions (up to 9 fractions without exchanging bottles)
· Subambient operation thanks to an integrated compressor (no need for liquid coolants)
The main steps in the preparative fractionation process (dissolution, column loading, crystallization, elution, and fraction collection) are automatic. There is no manual handling of hot solvents involved. There are two fractionation modes offered in its versatile software.
The TREF method is used in preparative fractionation by chemical composition in a column support. By exchanging the column, the fractionation can be performed by Thermal or Solvent Gradient Interaction Chromatography.
Molar Mass fractionation is based on the solvent interaction with the polymer chains and it is typically performed at isothermal conditions by modifying the solvent strenght through a solvent, non-solvent combination.
The incorporation of an optional IR4 detector is possible to ensure the column's proper rinsing after each fraction (recovery of the solvent baseline) in the compositional mode.
The PREP C20 Software automates the compositional and molar mass fractionation of the polymer. The PREP C20 software offers wide flexibility when setting the different conditions involved in the fractionation process: such as the number of fractions obtained, column loading volume, temperature steps or cleaning cycles.
PREP C20 user just needs to weight the sample, put it inside the vessel, select the fractionation conditions and start the software. From this point on, the instrument performs the vessel filling with solvent, dissolution, column loading, crystallization, elution and fraction collection.
The PREP C20 Software has been designed as a powerful Virtual Instrumentation interface to the instrument hardware, collecting all the sensors signals during the whole fractionation process as well as monitoring them in real-time, watching at the expected behaviors and warning the user about any abnormal issues during the fractionation.
A manual mode is also available in the PREP C20 Software, like in all Polymer Char’s instruments, as a very useful tool for diagnosis. As a result, every part of the instrument can be operated remotely. This manual mode in an equipment with IR4 is especially useful when fractionating unknown or difficult samples, allowing to perform step by step fractionations, which provides the user all the flexibility to adapt the fractionation conditions to the sample requirements.
PREP C20 is a fully-automated preparative pilot-plant-type equipment designed to fractionate, in a column support, high amounts of polymer according to its chemical composition by a Temperature Rising Elution Fractionation (TREF) process, or according to its Molar Mass, by modifying the solvent power through a solvent-non solvent combination, typically in isothermal conditions.
Yes, it provides the different fractions corresponding to the temperature steps selected.
No. PREP C20 is a preparative instrument. An IR4 detector can be incorporated optionally, however its purpose is to ensure the column proper rinsing after each fraction; no analytical result is provided.
Up to 20g of polymer, depending on the nature of the sample.
Unlimited number of fractions (up to 9 fractions without exchanging bottles).
No preparation of samples is required by the user other than weighing the dry sample and putting it inside of the vessel. The rest of the steps are performed by the instrument automatically: vessel filling, dissolution, column loading, fractions collection, final cleaning, etc.
After the automated fractionation process, fractions will be found separated in different glass vessels and mixed with solvent. By using any standard filtration system, fractions can be separated from the solvent and dried, to become ready to be weighed and analyzed by GPC, TREF, CRYSTAF, DSC, NMR, etc.
Solvents need to be handled only after the fractionation process, which is completely performed by the instrument.
After the automated fractionation process, fractions will be found separately in different glass vessels and mixed with solvent. By using any standard filtration system, fractions can be separated from the solvent and dried, to become ready to be weighted and analyzed by GPC, TREF, CRYSTAF, DSC, NMR, etc.
Any solvent compatible with viton o'rings and sealings can be used. To fractionate polyolefin samples, the solvents mainly used are TCB and oDCB. The non-solvent used is Diethylene Glycol Monobutyl Ether (DEGMBE).
PREP C20 has been used to fractionate polyolefin mainly, but any polymeric sample might be fractionated by using any compatible solvent. Please refer to the question above 'Which solvents can be used?' for more on this.
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