Overview
Two-dimensional chromatography analysis is performed by a Polymer Char’s Solvent Gradient Interaction Chromatography SGIC 2D Instrument, developed for a detailed study of the chemical composition – molar mass bivariate distribution of amorphous or low crystallinity polyolefins and functionalized polyolefins. Chemical composition separation is achieved by a gradient of solvents in an interaction chromatography column as a first dimension, followed by molar mass separation in a second dimension by isocratic Gel Permeation Chromatography (GPC) / Size Exclusion Chromatography (SEC).
3D and contour plots as well as the recovered 1st dimension SGIC and 2nd dimension GPC recovered profiles, are obtained with this 2-dimensional analysis.
In addition, the IR5 built-in detector can provide a direct measurement of chemical composition in polyolefins (methyls content, comonomer weight fraction)
A report is sent to the customer with the bivariate distribution graphs, single dimension recovered graphs, the analysis conditions used as well as tabular data with fractions average results.
The following are some results of analyses performed by SGIC 2D:
Analysis of two different heterogeneous PP copolymers by SGIC 2D
High impact PP copolymers are complex materials in which different fractions of ethylene-propylene copolymer of different composition together with homopolymer PP, mainly isotactic are found. Crystalline and amorphous fractions are mixed so interaction chromatography is required to achieve full separation of all existing components. The relative amount of each component as well as their composition and heterogeneity all can impact the final material properties.
With an SGIC 2D analysis the microstructure of such complex products is revealed so differences between samples can be detected, which can be related to process/catalyst as well as to properties. Both 3-dimensional, as well as contour plots, are useful to identify microstructure features and trends.
Method: Gradient decanol to TCB 100 min., Hypercarb® column, 1xrapid GPC column, Columns temperature: 160ºC, 2 minutes/fraction.
Isotactic polypropylene is weakly retained on the IC column while linear polyethylene retention is strong. Therefore blend components are easily separated, while the IR detector helps to unequivocally identify them by means of the observed methyl frequency (recovered 1st dimension profile with IR detection of methyl frequency).
The second dimension GPC analysis of the fractions provides useful information on the molar mass and molar mass distributions of the components of the blend (2D-contour plot).
Method: Gradient decanol to TCB 100 min., Hypercarb® column, 1xrapid GPC column, Columns temperature: 160ºC, 2 minutes/fraction.
Comonomer content in copolymer fractions varies the retention strength and therefore SGIC separation allows determination of chemical compulsion distribution in the case of heterogeneous copolymers. In the case of ethylene-propylene copolymers the retention strength increases (longer retention volumes) when the ethylene fraction increases. The online IR detector, connected after the isocratic second dimension) determines the ethylene content in each 1st dimension fraction. The observed ethylene content confirms the separation according to chemical composition and allows quantification of the distribution.
Method: Gradient decanol to TCB 100 min., Hypercarb® column, 1xrapid GPC column, Columns temperature: 160ºC, 2 minutes/fraction.
These detectors are used in our SGIC 2D analyses:
When analyzing HDPE pipe resins, high sensitivity is required to be capable of measuring the low number of branches accurately. IR5 detector was designed for this specific purpose and it is very powerful when characterizing that kind of resins.
The IR6 Detector is the latest IR Detector developed by Polymer Char with same capabilities and features than IR5 detector and the additional capability of measuring carbonyls group in the band of 1740 cm-1. IR6 Detector is recommended for users willing to analyze polyolefin type EVA, EBA, and others with carbonyls group present in IR band above.
| SGIC 2D (Price/Sample) | First Sample | Additional Samples |
| Standard | 1.396€ | 1.161€ |
| Additional Results: | 1.725€ | 1.394€ |
| Chemical Composition | 720€ | 598€ |
| Calibration for Chemical Composition | 214€ | 0€ |
| Additional Services: | ||
| Sample Filtration (carbon blak) | 204€ | 204€ |
| Standard Data Re-processing | 109€ | 109€ |
| Patent Interpretation | 300€ | |
| Minimum sample amount | >1 g |
The fractionation service is available thanks to the Instruments PREP mc2 and PREP C20, capable of fractionating samples by molecular weight or by composition (TREF or CRYSTAF). Please visit the link Preparative Fractionation for more information.
The resulting fractions are later analyzed by the corresponding technique (GPC or TREF/CRYSTAF) to check the good performance of the fractionation process. Finally, the physical fractions are sent back to the customer by courier service as well as the analysis results of the fractions, so the customer can check the separation.
For most of our analyses, you will receive a summary of the results along with an Excel file. However, the type of data and report form depends on the analytical service made. For specifics about the information sent, contact analyticalservices@polymerchar.com.
Please send an email to analyticalservices@polymerchar.com and we will be pleased to help you.
To order any analytical service, please fill in the Analytical Service Request Form. Provide all the information available about the samples to be analyzed. Sent forms will be processed as formal orders for Polymer Char records. All the information provided is considered confidential information.
If a previous quotation is required, please do not hesitate to let us know by sending an email to analyticalservices@polymerchar.com
Samples should be shipped to:
Polymer Characterization S.A.
Valencia Technology Park
Gustave Eiffel 8
Paterna, Valencia
E-46980, Spain
Attn.: Analytical Services Department
We highly recommend to use courier service instead of post mail to ensure your samples arrive in good condition.
You will receive the results in less than a week. If you plan to send more than 2 samples, please check with our lab, as the response time may be longer in this case.
This time is approximate, and it depends on the service queue in the laboratory at the time of the order. Polymer Char will inform the customer if the turnaround time is expected to be longer.
Please refer to our Analytical Services Terms and in the first chapter, you will find the necessary amount for each technique.
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Webinar Modern Separation Techniques
Date: November 2021
Speaker: Alejandro Fernández
Webinar ABPol
Date: March 2021
Speaker: Alberto Ortín
Published in The Column
Vol. 10, Issue10.
June 2014, Pages 20-24
B. Monrabal
Published in American Laboratory
January 2011
A. Ginzgburg, T. Macko, R. Brull
Published in: Macromolecular Chemistry and Physics 2013
Volume 214, Pages 2165-2171
Authors: S. Cheruthazhekatt, N. Mayo, B. Monrabal, H. Pasch.
Published in: Macromolecular Symposia. Polyolefin Characterization, ICPC 2012.
Volume 330, 2013, Pages 9-21, Wiley-VCH.
Authors: Benjamin Monrabal, Esther López, Loli Romero
Poster Presented at the 8th International Colloquium on Heterogenous Ziegler-Natta Catalysts
2012
Poster
Presented at Pitton
2011
These are the instruments used to obtain this analysis and others that might be of interest to you:
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