Spring 2007 Newsletter
Unlocking the Secrets of Deformulation
(reverse engineering)
Deformulation, also know as reverse engineering, is the use of analytical techniques to determine the chemical composition of a product or sample. Deformulations are performed for a variety of reasons such as investigating patent infringements, understanding why one product is outperforming another and to investigate a competitor’s product. These investigations can be performed on polymers, chemical formulations, composite materials and many other materials and products. The most difficult products to deformulate are those involving natural materials such as processed foods and herbal extracts.
The successful deformulation involves a strong understanding of the chemical properties of the class of materials in question such as polymers or surfactants. Before beginning, a detailed literature review of the materials should be conducted and used to create a plan for analysis. A good plan will include a strategy for successfully separating the constituent components of the sample so that the components can be identified and quantified accurately.
Combinations of several spectroscopic, chromatographic, and thermal techniques may be used to accurately identify and quantitate the material. These techniques include FT-IR, proton NMR, carbon NMR, GC, GC/MS, LC or HPLC, thermal analysis (TGA, DSC or MDSC), SEM/EDXA and ICP. The technique used depends on the property of the material and each gives unique insight into the material’s identity.
Once the data is collected, careful interpretation is key to disclosing the identity of the material in question. Often families of materials show similar analytical properties. Interpreting the small differences takes a combination of refined experience and attention to detail.
Since 1959, Chemir has deformulated several hundred polymeric products including thermoplastics, elastomers, composites, adhesives, sealants, inks, paints and coatings. These materials touch our lives daily and are the key components in consumer, industrial and medical products.
One example of a successful deformulation performed at Chemir involved the deformulation of several UV cure urethane acrylic oligomer based dental-filling products. FT-IR was performed in order to obtain basic information of the major components in the sample. NMR analysis was then performed and provided more accurate and detailed information about the major components previously identified by FT-IR. Next, solvent extraction was used to separate inorganic fillers from the organic fraction, and GC/MS analysis was performed to identify volatile and semi-volatile additives at low levels, such as monomers, chain extenders, antioxidants and photoinitiators. GC, GC/MS and HPLC then quantified the volatile and semi-volatile additives. The non-volatile polymers and high molecular weight oligomers, were positively identified and quantified based on NMR and solvent extraction data.
Once the molecular structures of the urethane-acrylate oligomers used in the UV cure dental filling products were successfully determined from the data acquired from the organic portion, we moved on to the inorganic portion. The inorganic fillers in the dental filling products were identified by SEM/EDXA, ICP and their FT-IR spectra.
Finally, our scientists interpreted the data collected and the results of our analysis were presented to the client in a clear and comprehensive report. Our interpretation of the data was praised by the client and was used to enhance their product development.