Deformulation
It is a multi-step process that requires a combination of physical separation techniques and advanced analytical methods. The goal is to break down a complex mixture into its individual components, identify each component, and determine their relative concentrations. This process is essential for understanding the composition of industrial products, ensuring quality control, and facilitating reverse engineering efforts.
The use of multiple instruments and techniques ensures that a wide range of components, from inorganic salts to complex polymers and surfactants, can be accurately identified and quantified.
This process is crucial for quality control and regulatory compliances. Below is a detailed explanation of the steps and techniques involved in deformulation:
Separation of Components
Residue Analysis: After extraction, the remaining residue typically contains water-insoluble fillers.
Centrifugation: Heavier fractions like fillers are separated using centrifugal apparatus. This is particularly useful for separating components based on density differences.
Solvent Extraction: Different solvents of varying polarity are used to extract specific components. For example:
Alcohol Extraction: Surfactants like linear alkyl benzene sulfonate (LAS) or sodium lauryl ether sulfate (SLES) can be extracted using alcohol.
Water Extraction: Inorganic salts such as sodium tripolyphosphate (STPP), sodium sulfate, or sodium chloride are extracted using water.
Acid Treatment: Addition of a mineral acid can help separate organic acids from the mixture.
Identification
X-Ray Fluorescence (XRF): Used for elemental analysis, particularly for identifying inorganic components like fillers and salts.
Fourier Transform Infrared Spectroscopy (FTIR): Used to identify functional groups and molecular structures of the separated components.
Nuclear Magnetic Resonance (NMR): Provides detailed information about the molecular structure, including the arrangement of atoms within a molecule.
Direct Mass Spectroscopy (MS): Helps in identifying the molecular weight and structure of the components.
Analysis
Pyrolysis Gas Chromatography-Mass Spectrometry (Pyrolysis-GCMS): Polymers are often copolymers made from more than one monomer. Pyrolysis-GCMS involves heating the polymer until it decomposes into smaller molecules, which are then analyzed by GCMS.
Pyrolysis: The polymer is heated to high temperatures, causing it to break down into monomers or other small molecules.
GCMS Analysis: The volatile decomposition products are analyzed using GCMS, which has a large library of compounds to help identify the monomers or their decomposed products.
Non-Ionic Surfactants: These typically give identifiable peaks in GCMS, allowing for the identification of the hydrophobe (the non-polar part of the surfactant molecule).
Solvent Dissolution: Surfactants are dissolved in a solvent like methanol before analysis.
GCMS Analysis:
Sulfates and Sulfonates: Compounds like SLES or linear alkyl benzene sulfonate (LAS) may not give clear peaks in GCMS.
Integration of Data
Report Generation: A comprehensive report is generated, detailing the composition of the formulated product, including the identity and concentration of each component.
Cross-Referencing: Data from different techniques (FTIR, NMR, MS, XRF, GCMS) are cross-referenced to ensure accurate identification and quantification of all components.
Precision analytics 