A reliable and fully-automated instrument for amorphous phase determination in PP/EP Manufacturing QC laboratories
A reliable and automated instrument for Amorphous Fraction determination in Quality Control laboratories of Polypropylene plants.
Based on the Crystaf for Extractables (CRYSTEX) technique, CRYSTEX® QC is a step forward in technology for automating the Soluble Fraction determination (amorphous fraction) in polypropylene and other polyolefin resins. This is a reliable instrument for continuous operation in the manufacturing plant laboratory, with minimum bench-space and utilities requirements.
CRYSTEX® QC stands as a modern alternative to the traditional gravimetric or wet chemistry method based on xylene solubility. The results obtained in CRYSTEX® QC show an excellent correlation with the classic gravimetric method while obtaining better reproducibility thanks to its full automation. In contrast, the gravimetric analysis is known for being very time consuming, and for requiring constant manual handling of solvent at high temperature. In comparison, CRYSTEX® QC is very easy to operate, and obtaining the amorphous phase content in a shorter time. It also eliminates the need to handle solvent manually and it uses less-flammable solvents than Xylene (TCB or oDCB), increasing the safety level in the laboratory.
The only manual task required is to put a representative amount of sample (up to 4g) in a disposable bottle, without the need for accurate weighing. The instrument then automates the entire analysis process, including dissolution, separation of the soluble fraction from the crystalline matrix, and analysis by the online detectors. This whole process takes 2.5 hours, and thanks to its self-cleaning capability, the instrument is then ready for the next sample analysis.
The crystalline and amorphous fractions are separated through a crystallization and re-dissolution temperature cycle within a proprietary TREF column. Precise quantification is achieved by means of an infrared detector that also delivers ethylene content information. Moreover, the instrument measures intrinsic viscosity by means of a built-in dual capillary viscometer. All results (concentration, ethylene content, and intrinsic viscosity) are obtained for the whole sample, the amorphous fraction, and the crystalline fraction.
A Fully-automated analysis of multiple samples (up to 42), known to be homogenous (pelletized), can be performed using the same technology in the CRYSTEX® 42.
· Fully-automated analysis of the soluble (amorphous) fraction in polypropylene and other polyolefins
· A sample can be analyzed every 2.5 hours (including dissolution and rinsing time) without manual operation
· No need for accurate weighing of sample nor manual solvent handling
· No external filtration nor solvent evaporation required
· Additional measurement of ethylene content and intrinsic viscosity for the fraction, the crystalline fraction, and whole sample
· For Process /QC laboratories in production plants
· Compatible with other polyolefin materials such as LDPE, and adaptable to other solubility tests (heptane or hexane solubles)
· Excellent correlation between CRYSTEX QC results and the traditional xylene solubles ISO/ASTM methods
The following are the detectors available for CRYSTEX® QC
The IR4 is the standard Detector integrated by default in all the Polymer Char analytical instruments. IR4 is a dual-wavelength infrared detector, which uses the principle of infrared absorption spectroscopy to measure the concentration and composition in polyolefins.
Polymer Char offers a highly sensitive Two-Capillary Relative Viscometer. Both options are an ideal complement to the infrared detection systems implemented in many of the polyolefin characterization instruments, such as GPC-IR or CEF. Viscometer configuration is optimized to achieve a better performance in each technique.
CRYSTEX® QC is controlled by an intuitive and easy-to-use software that automates the analytical process and provides tools for instrument maintenance and advanced operations.
Two operation modes are available in the CRYSTEX® QC software: Operator and Administrator. In the Operator Mode, the software allows routine analysis to be performed using the pre-defined Soubles Method, and the results are automatically generated in a report. Therefore, starting a run only involves putting the pellets or powder inside the analysis bottle and starting the software. In about 2,5 hours, the whole analytical process will be completed, including sample dissolution and analysis. The Results Report is automatically produced on the computer screen. The software has been built as a Virtual Instrument that allows the operation of the hardware parts from the computer and the reception of feedback from all the actions and the detectors’ signals.
The user doesn’t need to work manually at a high-temperature nor handle solvents during any maintenance or diagnosis tasks. For all the data processing, the GPC One Software package is used. This software provides the calibration methods, and the results and calculations. The results from all the analyzed samples are stored in separate files in the computer’s hard disk and organized in folders for convenient management of all the historical data.
The Xylene Solubles percentage is directly provided, as well as the concentration measured by the infrared detector; thus, there is no need for accurate sample weighing before starting the process. When additional detectors are incorporated into the CRYSTEX® QC equipment, intrinsic viscosity results and ethylene (C2) content will be shown per sample as well, both for the parent sample and for the amorphous and crystalline fractions.
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These two instruments automate the technique of the Xylene Solubles test. They are intended to measure the amorphous fraction of polypropylene and ethylene-propylene copolymers. The accuracy and precision of the Xylene Solubles test are very important to the process and product specifications of the resultant materials.
Traditionally, this test has been done using the gravimetric method, which requires manual operation along the whole process. As a result, the precision is poor and the procedure is time consuming and not safe.
Polymer Char’s CRYSTEX 42 and CRYSTEX QC instruments automate this technique obtaining high precision and accuracy in the results as well as avoiding manual solvents handling.
While CRYSTEX® QC was designed to be installed in each production plant to monitor in real time the process or the grade changes analyzing a significant amount of powder sample (up to 4 grams), CRYSTEX® 42, thanks to the incorporation of a high temperature autosampler with 42 positions, becomes a perfect complement to be used in a central lab, where large batches of pelletized more homogeneous samples need to be analyzed.
Yes, they are.
CRYSTEX® 42 and CRYSTEX® QC are analytical instruments designed to measure the Soluble Fraction percentage in a fully automated way, but they don't provide any physical fraction. For this purpose, please read about PREP mc2 or PREP C20.
Up to 42 samples can be run by the CRYSTEX® 42 autosampler. Dissolution and full analysis of the first sample completed in three hours. For the subsequent samples, it takes about two hours.
One sample is performed in each run and complete process, including dissolution is carried out in about 2.5 hours.
The standard amount used in CRYSTEX® 42 analysis is around 160mg per sample and in CRYSTEX® QC is 2g.
Due to the fact that the exact concentration is measured by the infrared detector during the analysis, there is no need of using the balance at all. Up to half a gram can be used for overcoming sample heterogeneity issues.
1,2,4-Trichlorobenzene (TCB) and Orto-Dichlorobenzene (oDCB) are the most used solvents. To use other solvents please consult Polymer Char first.
Yes, both obtain the Soluble Fraction without the use of xylene. It has been shown that there is a good correlation between soluble fraction measured in Xylene or in other solvents. Therefore, by applying the proper calibration, results obtained in other solvent can be translated to Xylene.
No samples preparation is required by the user but putting the dry samples inside the vials in case of CRYSTEX® 42 and in the bottle in case of the CRYSTEX® QC (weighing doesn’t need to be precise). The rest of the steps are performed by the instrument automatically: vials filling, dissolution, crystallization, final cleaning, etc. Therefore, when a sample analysis is finished, another one can be followed immediately.
Solvents don’t need to be handled at any time; the whole process is fully automated, the instrument is in charge of all the needed steps: vials filling, dissolution, crystallization, final cleaning, etc.
This instrument is specially designed for the determination of the Soluble Fraction in polypropylene resins but it can be used for polyethylene as well.
CRYSTEX® 42 and CRYSTEX® QC incorporate an infrared detector to measure the concentration of the solution both at high temperature when the sample is 100% dissolved and also at room temperature, to measure the percentage of the sample which remains in the solution after the crystallization cycle (rubber content). This detector is Polymer Char’s IR4 in its OEM version and therefore a composition sensor could be incorporated as well, to measure the methyls or carbonyls content on the whole sample and on the amorphous fraction.
A capillary viscometer and/or a composition sensor can be coupled to CRYSTEX® 42 or CRYSTEX® QC without adding complexity to the process. Therefore, additional information about the intrinsic viscosity and/or ethylene content on the whole sample and on the rubber content can be obtained with a similar analysis time.
For all the data processing, the GPC One Software package is used. This software provides the calibration methods, the results, and calculations. Results will provide directly the XS% per sample as well as the concentration measured by the infrared detector, as a result, there is no need for an accurate sample weighing before the process.
When additional detectors are incorporated into the instrument equipment, intrinsic viscosity results and methyls content will be shown per sample as well, both from the whole sample and also from the rubber content percentage.
The soluble fraction results of CRYSTEX QC show an excellent correlation compared to those obtained with the xylene solubles ISO/ASTM methods for a wide selection of PP resins, but CRYSTEX QC has better reproducibility thanks to the automation of the system. Moreover, CRYSTEX QC shows a standard deviation (std) of less than 0.1%, much lower than indicated by the standard methods.
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