Deformulation of polymers in the laboratory
Reminder : deformulation, what are we talking about?
Deformulation, or otherwise known as “reverse engineering”, consists in determining the nature and quantities of materials present in a formulation. In short, it consists in analyzing and fragmenting the chemical composition of a product.
This process is used in various contexts…
- To analyze and determine the composition of an unknown mixture,
- To compare the composition of several products (double-sourcing or multi-sourcing),
- Checking the conformity of a product to a Safety Data Sheet (SDS) or a technical data sheet,
- Understand an unusual phenomenon, etc.
… and applies to all types of industrial sectors: pharmaceutical formulations, cosmetics, chemicals, paint, etc.
FILAB has also set up deformulation services adapted to solids (powders, metal alloys, ceramics, etc.), and more particularly to the world of polymers, which have a wide variety of formulations.
FILAB: a service dedicated to deformulation of polymers
With a wide range of analytical equipment and human skills in the field of polymers, FILAB has developed a service offer dedicated to the deformulation of polymers (PE, PP, PET, PVC, etc.) and polymer-based formulations (paints, varnishes, silicones, etc.), including chemical, physical and thermal analysis.
Some analysis will be performed directly on the sample or on a specific preparation after extraction in a solvent, with the objective of isolating the mineral fraction and the organic fraction for better interpretations. Depending on the context and your objectives, our team will propose the most appropriate techniques.
Determination of the phases mineral
Determination of the decomposition temperatures of the polymer, as well as its percentage of mineral fillers. A verification of the presence of carbon black can also be done with this technique
The SEM equipped with an EDX microprobe allows morphological observations and local semi-quantitative chemical analysis of the polymer fillers.
The XRD determines the nature of the crystalline phase(s) constituting the polymer fillers.
The ICP-AES analysis is performed after mineralization of the sample and will be used to determine the chemical composition of the mineral fillers
Determination of the phases organic
FTIR is often the preferred technique for determining the chemical nature of the sample’s constituent bonds. A spectral search in our data library is then performed to identify the polymer family present.
Determination of the glass transition temperature of different families of polymers. It also allows to determine if the polymer is semi-crystalline or amorphous.
Pyrolysis-GC allows to degrade the sample, to go back to its chemical structure. It allows to highlight the presence of residual solvents and/or residual monomers, the constituent monomers and the presence of additives.
The GCMS Screening, in addition to the pyrolysis, also identifies the polymer additives, the polymeric chains present, as well as the presence of cyclosiloxanes (D3, D4, D5?).
The GC-FID allows to quantify the different extractable agents and additives present in a rubber formulation. The analysis is performed after specific preparation on the organic phase.
Identification and quantification of compounds contained in the extractives.
Thanks to its database of more than 2000 substances, the LC-QTOF is used to search for additives present in the polymer, or to identify unknown impurities.
All results are then combined and interpreted according to the client’s context.
Also, other analytical techniques can, depending on the matrix, be relevant in deformulation processes such as: GPC (molecular weight measurement and chain length distribution study), NMR (structural analysis), etc.
As an independent laboratory, with a team of experienced doctors and engineers, FILAB guarantees the reliability of its results, ensures rapid processing of requests and provides personalized support to its customers.
Some examples of cases conducted at FILAB:
Faced with increasingly regular raw material supply problems, our client wanted to have more information on the HDPE in question in order to be able to establish precise specifications and find other potential suppliers. In this perspective, our objective was to obtain the maximum of physicochemical data on the polymer. The analysis implemented were: TGA, SEM, DSC, FTIR, Py-GCMS and density measurements.
Our client was working on heritage materials and in particular on the conservation of old objects. Here, we were asked to learn more about the composition of the paints used at the time in order to adapt the conservation processes. In this case, we focused on the organic part of the paint with studies by µ-IRTF, a research of solvents by GCMS and a more detailed study by Py-GCMS with 3 heating levels.
Within the framework of the development of a new product, our customer wished to compare several materials from different suppliers in order to identify the physico-chemical properties most in adequacy with the final use of the product. Here, we were initially interested in the research of fillers and additives with FTIR, Py-GMCS and ATG.
The context here was that of an abnormal and unusual adhesive non-performance (adhesion problem). Here, comparative deformation between a compliant and a non-compliant sample revealed the presence of impurities in the non-compliant sample.
Our client was looking to deform a so-called “biodegradable” plastic bag used for coffee packaging. The goal was to know if the plastic was indeed composed of a biodegradable polymer, PLA (polylactic acid). For this purpose, FTIR analysis was proposed because PLA has specific bands that allow us to conclude on its presence. However, the bands of PLA can potentially hide the bands of other polymers (polyethylene for example), so another method, the DSC (dynamic scattering calorimetry) was also proposed. Indeed, the temperatures are different depending on the nature of the polymers present.
Polymer deformulation is useful in many cases, particularly for analysing the properties of polymers used in the manufacture of products. It can help to determine :
the chemical composition of a polymer material
its molecular weight,
its thermal stability,
fracture toughness,
and durability in various environments.
This information can be useful in many technical areas, such as product quality, production control, research and development of new products, and failure analysis. Specifically, polymer deformulation provides essential information for understanding and improving the performance and quality of polymer products.
