A reliable and automated instrument for intrinsic viscosity analysis of polymeric materials
Fully-automated instrument for determination of intrinsic viscosity in polymeric materials.
Polymer Char introduces the Intrinsic Viscosity Analyzer (IVA) in response to the market’s need for a reliable and automated instrument for Intrinsic Viscosity (IV) analysis of polymeric materials in solution. Intrinsic viscosity can be seen as an indirect measurement of the average molar mass and, as a result, it provides valuable information within any polymer characterization process. IVA is based on Polymer Char’s recently developed QC platform, which integrates, in a reduced footprint, a robust dual-capillary relative viscometer combined with a high-temperature autosampler with a capacity for 42 samples. IVA can analyze a wide range of polymers with IV values from 0.5dL/g up to over 40dL/g, such as polyolefins, PET, PAN, PMMA, and others, by using almost any organic solvent. For each of these polymers that have been tested, all of the Intrinsic Viscosity results are in good agreement with the traditional methods of reference (compared to the IV obtained with glass capillaries or the Ubbelohde type. ISO 1628-3:2010 f.i.).
When using IVA, the analyst places the vials with polymer into the autosampler’s external tray, at room temperature. Then the instrument takes the vials into the dissolution oven, fills them with solvent and starts shaking. Dissolution temperature, shaking intensity, non-oxidative atmosphere with nitrogen, and time are accurately controlled so that the analyst can select the optimum conditions to achieve full dissolution while minimizing thermal degradation.
The analysis of polyolefins and other polymers containing significant C-H content can be further improved by the incorporation of the optional Infrared detector IR4 to accurately quantify the injected polymer’s mass, which results in improved precision and accuracy of intrinsic viscosity determination.
The IVA capillaries and tubing do not require manual washing or rinsing and provide robust and precise viscosity values over time. The careful design of the heated compartment and transfer lines ensure that no cold spots are found and that even the most challenging polymers can be analysed.
· Full-automation of dissolution and analysis processes. No manual solvent handling
· No need for accurate weighing when the optional IR detector is used
· High-temperature autosampler for dissolution of samples in the same instrument
· Self-cleaning design based on dual capillary relative viscometer
· Simple to operate and reliable instrument
· High precision achieved by automation
· Up to 42 samples can be analyzed sequentially without user intervention
· Analysis of high and ultrahigh molar mass polymers
· Low solvent consumption
· Compatible with most organic solvents such as decaline, chloroform, tetrahydrofuran, tri-chlorobenzene, and others
· Excellent correlation IV results with the traditional glass capillary system of the Ubbelohde type for different polymers
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.
IVA 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 IVA software: Operator and Administrator. In Operator mode, the software allows routine analysis to be performed using the pre-defined Method, and results are automatically generated in a Results Table. Therefore, starting a run only involves putting the pellets or powder inside the analysis bottle and starting the software. In about 2 hours, the whole analytical process will be completed, including sample dissolution and analysis, and a Results Table is automatically generated on the computer screen. In Administrator mode, apart from the Operator mode functions, the analytical and data processing conditions can be optimized, calibration methods are available as well as review and re-processing of previously analyzed files.
Results from all the analyzed samples are stored in separate files in the computer’s hard disk and organized in a Data Base for convenient management of all the historical data. Intrinsic Viscosity value is directly provided, as well as the concentration measured by the infrared detector (optional detector); thus, there is no need for accurate sample weighing before starting the process.
The IVA Software incorporates a manual mode to be operated by the Administrator or by Polymer Char engineers. This manual mode becomes a powerful tool since it functions as a Virtual Instrumentation interface for the instrument hardware to perform any action on any hardware element. Consequently, the user does not need to work manually at a high temperature nor handle solvents during maintenance or diagnosis tasks.
The purpose of the IVA (Intrinsic Viscosity Analyzer) is the analysis of the intrinsic viscosity of polymeric materials in solution.
Intrinsic viscosity can be seen as an indirect measurement of the average molar mass and, as a result, it provides valuable information within any polymer characterization process.
Up to 42 vials can be handled by the IVA autosampler, and they can be dissolved and analyzed, and no supervision is required. Total time will depend on the dissolution time and number of injections per vial. Each injection of each vial will last the programmed analysis time, typically 15 minutes. Only the dissolution time of the first sample should be added to this total time, as the dissolution of the following sample will be carried out while the previous sample is being analyzed.
Between 4 and 16mg are used as the standard for preparing a 0.25 to 1mg/mL solution in the autosampler vial.
The equipment is compatible with most organic solvents.
The solvent used will depend on the polymer to be analyzed as the polymer has to be in solution for the analysis.
PE, PP, EP, UHMWPE:
Decaline, trichlorobenzene, orto-dichlorobenzene.
Mixtures of phenol:TCE and phenol:orto-dichlorobenzene.
IVA instrument can be used from room temperature to 180ºC, depending on the polymer and solvent to be analyzed.
The analysis and dissolution temperature are independent, so different temperatures can be used for each step.
No samples preparation is required by the user but weighing the dry samples and putting them inside of the disposable glass vials. The rest of the steps are performed by the instrument automatically: solvent filling into the vials, dissolution, injection, etc.
As the samples are being analyzed, a summary table with the automatic calculations generated with the processing software GPC One is shown.
The user has always the possibility of validating the results generated automatically with the GPC One software.
A reporting tool has also been developed, generating reports in Excel adapted to each user needs.
The IV analyses provided by the IVA instrument are very reliable. All the IV results have shown a very good correlation when compared to the IV obtained using the traditional Ubbelohde type glass capillary system. We have tested different polymers in various solvents, and all resulted to be in accordance with the method of reference (ISO 1628-3:2010 f.i.)
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