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PRODUCT DEFORMULATION AND REVERSE ENGINEERING

There are many reasons for which a client may need product deformulation services.  Examples include the desire to learn about a competitor’s product for purposes of reverse engineering, the need to assess whether a competitor may be infringing on one’s composition of matter patents, and even the need to learn about the details of one’s own product so that one can continue manufacturing it after the death of a key employee who knew all the details but did not keep comprehensive and up to date records.

Deformulation

Deformulation services may be needed for any type of polymeric product; such as a one-part or two-part liquid formulation that will be cured into an epoxy, urethane, or acrylic adhesive; a thermoplastic or thermoset (co)polymer of any composition and molecular architecture and possibly including any of a wide variety of additives; and both conventional composites and nanocomposites using such (co)polymers as their matrix materials.

The experimental techniques that may be used in a deformulation project include, but are not limited to, liquid chromatography-mass spectrometry (LC-MS), high-performance liquid chromatography (HPLC), gas chromatography-mass spectrometry (GC-MS), inductively coupled plasma-mass spectrometry (ICP-MS), nuclear magnetic resonance (NMR), Fourier-transform infrared spectroscopy  (FTIR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), optical microscopy (OM), energy-dispersive x-ray spectroscopy (EDX), wide-angle x-ray scattering (WAXS), dynamic light scattering (DLS), equilibrium swelling measurements, differential scanning calorimetry (DSC), and thermogravimetric analysis (TGA).

It is obviously unnecessary to use all of these techniques in deformulating any given product.  The selection of appropriate techniques depends on the type of product that is being deformulated and the level of detail that needs to be explored for that product.

Most deformulation projects require some separation of the components within the sample.  LC-MS is used routinely to separate and identify less volatile components in a mixture, while GC-MS is used routinely to identify the more volatile components in the mixture. LC-MS and GC-MS provide mass information regarding the liquid and volatile components, respectively, in the sample.  Once these components are identified, followup chromatography experiments may be performed relative to standards for the major components, if desired, to quantify these components.

Other techniques are also used, as needed, to perform a complete deformulation.  For example, NMR and FTIR are used in most deformulations to probe into the details of the chemical composition and molecular structure, microscopy is useful in understanding heterophasic and/or textured products and the most useful type(s) of microscopy is (are) determined by the scales of the phasic and/or textural features (but the use of SEM is most common), EDX is often used for elemental analysis, WAXS is used if the sample is known to be crystalline or semicrystalline and detailed information is desired regarding the crystalline structure, DLS may be used to determine the size distribution of particles dispersed in fluids, equilibrium swelling may be used to measure the extent of cross-linking in a thermoset sample, and the use of DSC and/or TGA may provide additional valuable information in many deformulations.

A deformulation project normally comprises at least two stages.  The first stage provides very valuable and detailed but usually not comprehensive and fully quantitative information about the composition and morphology.  The second stage (and sometimes further stages) focus on building a more comprehensive and quantitative understanding of the product.  The point of diminishing returns is reached when the cost of pursuing an additional stage of deformulation is no longer justifiable in terms of the benefits of the additional details that will be learned.  Hence the deformulation project is ended when enough has been learned to provide a good starting point for the reverse engineering of the product or to make a sound judgment about whether patent infringement has occurred.

Call Bicerano & Associates Consulting, LLC at (912) 235-2238 or use our online form or email us at info@polymerexpert.biz today!

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