Deformulation

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Deformulation refers to a set of analytical procedures used to separate and identify individual components of a formulated chemical substance. [1] [2] [3] [4] Deformulation applies methods of analytical chemistry and is often used to obtain competitive intelligence about chemical products. Deformulation is related to reverse engineering; however, the latter concept is most closely associated with procedures used to discover working principles of a device or a designed system through examination and disassembly of its structure. The term, reverse engineering, has become specifically and almost exclusively linked to the field of software engineering; [5] [6] whereas, deformulation is a term more applicable to the field of chemical manufacturing. Deformulation of a multicomponent chemical mixture may occur in several contexts, including the investigation of causes of chemical product failure, competitive benchmarking, legal inquiry to obtain evidence of patent infringement, or new product research and development. Depending upon this context and upon the level of information sought, the requirements of analyses for deformulation may differ. [7] Deformulation processes typically require the application of several analytical methods, and the selection of methods is dependent upon the degree of confidence required in the results. Methods of deformulation also have similarity to methods of forensic chemistry in which analytical procedures may be applied to discover the causes of material failure or to resolve a legal question.

Analytical chemistry study of the separation, identification, and quantification of the chemical components of materials

Analytical chemistry studies and uses instruments and methods used to separate, identify, and quantify matter. In practice, separation, identification or quantification may constitute the entire analysis or be combined with another method. Separation isolates analytes. Qualitative analysis identifies analytes, while quantitative analysis determines the numerical amount or concentration.

Competitive intelligence (CI) is the action of defining, gathering, analyzing, and distributing intelligence about products, customers, competitors, and any aspect of the environment needed to support executives and managers in strategic decision making for an organization.

Reverse engineering, also called back engineering, is the process by which a man-made object is deconstructed to reveal its designs, architecture, or to extract knowledge from the object; similar to scientific research, the only difference being that scientific research is about a natural phenomenon.

Contents

In The United States, federal law recognizes a legal practice for the study of an item in hopes of obtaining a detailed understanding of the way in which it works for the purpose of creating duplicate or superior products without the benefit of having the plans for the original item. The studied item must first have been legally obtained, not stolen or otherwise misappropriated. [8] The purpose of intellectual property protection is to provide incentives to invest and to advance the collective knowledge. It is felt that deformulation or reverse engineering helps to educate and promote healthy competition. It is considered to be a learning tool which provides a path to making new, competitive products that perform better and at lower cost than what is currently on the market. Deformulation is often considered along with benchmarking, patent mapping, and other competitor intelligence gathering processes as a means of conducting day-to-day business. [9]

Other countries may have different conceptions about intellectual property rights and about legal allowances for deformulation or reverse engineering of items. For information concerning the legal status of deformulation practices in other countries throughout the world it is advisable to consult with an expert on intellectual property law.

Deformulation procedures

A preliminary zeroth order analysis may be performed to answer fundamental questions about the nature of the unknown material. Methods that might be used for the preliminary analysis include spectroscopic methods, such as infrared spectroscopy or x-ray fluorescence spectroscopy. The results of the zeroth order characterization of the material inform subsequent choices in later stages of analysis.

A formulated chemical mixture may contain multiple phases, such as suspended or emulsified material. A first-order analysis of the material may involve the separation of phases. Centrifugation, extraction, and filtration are examples of methods which separate material in different phases. Centrifugation is effective to separate phases that differ in density. Extraction is effective to separate immiscible liquid phases. Filtration is effective to separate dispersed particles that are sufficiently large in size to be trapped in a filter. This initial separation may require the selection of appropriate solvents to either dissolve solid components or to act as a diluent for liquids. The quantitative determination of phases is often determined gravimetrically.

Centrifugation is a technique which involves the application of centrifugal force to separate particles from a solution according to their size, shape, density, viscosity of the medium and rotor speed. This process is used to separate two miscible substances, but also to analyze the hydrodynamic properties of macromolecules. More-dense components of the mixture migrate away from the axis of the centrifuge, while less-dense components of the mixture migrate towards the axis, i. e., move to the center. Chemists and biologists may increase the effective gravitational force on a test tube so as to more rapidly and completely cause the precipitate (pellet) to gather on the bottom of the tube. The remaining solution (supernatant) may be discarded with a pipette.. Centrifugation of protein solution, for example, allows elimination of impurities into the supernatant.

Filtration process that separates solids from fluids

Filtration is any of various mechanical, physical or biological operations that separates solids from fluids by adding a medium through which only the fluid can pass. The fluid that passes through is called the filtrate. In physical filters oversize solids in the fluid are retained and in biological filters particulates are trapped and ingested and metabolites are retained and removed. However, the separation is not complete; solids will be contaminated with some fluid and filtrate will contain fine particles. Filtration occurs both in nature and in engineered systems; there are biological, geological, and industrial forms. For example, in animals, renal filtration removes waste from the blood, and in water treatment and sewage treatment, undesirable constituents are removed by absorption into a biological film grown on or in the filter medium, as in slow sand filtration.

Once separated, each material phase is itself a chemical mixture to be further analyzed. A second-order analysis of each phase will typically involve a selection among available analytical methods to further separate these components. Analytical methods used on liquid phases might include distillation or one of a variety of chromatographic separation methods. Distillation separates the components of a liquid mixture according to differences in their boiling points. Chomatography separates components of a liquid or gaseous mixture according to differences in retention time as the mixture interacts with a stationary phase. Individual components thus separated can then be identified by a variety of detection methods, including infrared spectroscopy, Raman spectroscopy, mass spectrometry, and nuclear magnetic resonance spectrometry. Methods used to further analyze solids might include thermal analysis (such as thermogravimetric analysis or differential scanning calorimetry), x-ray diffraction to characterize crystalline solids, microscopy, pyrolysis, combustion analysis, or surface spectroscopic methods.

Distillation method of separating mixtures based on differences in volatility of components in a boiling liquid mixture

Distillation is the process of separating the components or substances from a liquid mixture by using selective boiling and condensation. Distillation may result in essentially complete separation, or it may be a partial separation that increases the concentration of selected components in the mixture. In either case, the process exploits differences in the relative volatility of the mixture's components. In industrial chemistry, distillation is a unit operation of practically universal importance, but it is a physical separation process, not a chemical reaction.

Infrared spectroscopy

Infrared spectroscopy involves the interaction of infrared radiation with matter. It covers a range of techniques, mostly based on absorption spectroscopy. As with all spectroscopic techniques, it can be used to identify and study chemical substances. Samples may be solid, liquid, or gas. The method or technique of infrared spectroscopy is conducted with an instrument called an infrared spectrometer to produce an infrared spectrum. An IR spectrum can be visualized in a graph of infrared light absorbance on the vertical axis vs. frequency or wavelength on the horizontal axis. Typical units of frequency used in IR spectra are reciprocal centimeters, with the symbol cm−1. Units of IR wavelength are commonly given in micrometers, symbol μm, which are related to wave numbers in a reciprocal way. A common laboratory instrument that uses this technique is a Fourier transform infrared (FTIR) spectrometer. Two-dimensional IR is also possible as discussed below.

Raman spectroscopy spectroscopic technique used to observe vibrational, rotational, and other low-frequency modes in a system

Raman spectroscopy ; named after Indian physicist C. V. Raman) is a spectroscopic technique typically used to determine vibrational modes of molecules, although rotational and other low-frequency modes of systems may also be observed. Raman spectroscopy is commonly used in chemistry to provide a structural fingerprint by which molecules can be identified.

In some contexts further stages of analysis of the separated components may be required. The active ingredients of a formulated chemical product that differentiate it from another similar material may include proprietary ingredients or specific functional additives. [10] Such ingredients that play a key role in the performance of the material in an application may require a third-order analysis to more completely characterize them. Some examples of functional additives include surfactants, emulsifiers, dispersants, adhesion promoters, leveling agents, dyes and pigments, antioxidants, preservatives, and optical brighteners. Practically every type of chemically formulated product is associated with its own formulary of likely functional additive choices that can fulfill some critical role in performance. Deformulation may thus require both a breakdown of material composition and also identification of the functional role of key ingredients.

Examples of chemical product types and functional additive types

Formulated chemical productPossible functional additivesReferences
Laundry detergentsurfactants, bleaching agents, defoamers, enzymes, corrosion inhibitors, fragrances, thickening agents [11]
Offset lithographic inkdriers, waxes, antioxidants, rheology modifiers, lithography additives [12] [13]
Interior house paintpigments, extenders, initiators, chain transfer agents, coalescing agents, wetting agents, freeze-thaw stabilizers [14] [15]
Laminating adhesivecolloidal stabilizer, anionic surfactants, nonionic surfactants, chain transfer agents, plasticizers, humectants [16]
Automotive engine oilpour point depressants, viscosity modifiers, anti-oxidants, detergent inhibitors, anti-wear additives, friction modifiers [17]
Solder maskphotoinitiators, reactive diluents [18]
Carbonated beveragepreservatives, acidulants, sweeteners [19]

The analytical determination of a functional additive has particular problems associated with it. The concentration of a functional additive may be low compared to other ingredients; therefore, it may be difficult to detect. Proprietary ingredients are especially difficult to correctly identify. The functional role of a key component may not be obvious upon inspection. A key ingredient may be undisclosed by the maker of the material, but rather kept as a trade secret. Careful study of trade literature and patent filings associated with the manufacturer may aid the analyst in the characterization.

A trade secret is a type of intellectual property in the form of a formula, practice, process, design, instrument, pattern, commercial method, or compilation of information that is not generally known or reasonably ascertainable by others, and by which a person or company can obtain an economic advantage over competitors. In some jurisdictions, such secrets are referred to as confidential information.

Related Research Articles

Chromatography is a laboratory technique for the separation of a mixture. The mixture is dissolved in a fluid called the mobile phase, which carries it through a structure holding another material called the stationary phase. The various constituents of the mixture travel at different speeds, causing them to separate. The separation is based on differential partitioning between the mobile and stationary phases. Subtle differences in a compound's partition coefficient result in differential retention on the stationary phase and thus affect the separation.

An emulsion is a mixture of two or more liquids that are normally immiscible. Emulsions are part of a more general class of two-phase systems of matter called colloids. Although the terms colloid and emulsion are sometimes used interchangeably, emulsion should be used when both phases, dispersed and continuous, are liquids. In an emulsion, one liquid is dispersed in the other. Examples of emulsions include vinaigrettes, homogenized milk, and some cutting fluids for metal working.

Physical chemistry is the study of macroscopic, atomic, subatomic, and particulate phenomena in chemical systems in terms of the principles, practices, and concepts of physics such as motion, energy, force, time, thermodynamics, quantum chemistry, statistical mechanics, analytical dynamics and chemical equilibrium.

High-performance liquid chromatography method

High-performance liquid chromatography is a technique in analytical chemistry used to separate, identify, and quantify each component in a mixture. It relies on pumps to pass a pressurized liquid solvent containing the sample mixture through a column filled with a solid adsorbent material. Each component in the sample interacts slightly differently with the adsorbent material, causing different flow rates for the different components and leading to the separation of the components as they flow out of the column.

Thermal analysis is a branch of materials science where the properties of materials are studied as they change with temperature. Several methods are commonly used – these are distinguished from one another by the property which is measured:

Chemometrics is the science of extracting information from chemical systems by data-driven means. Chemometrics is inherently interdisciplinary, using methods frequently employed in core data-analytic disciplines such as multivariate statistics, applied mathematics, and computer science, in order to address problems in chemistry, biochemistry, medicine, biology and chemical engineering. In this way, it mirrors other interdisciplinary fields, such as psychometrics and econometrics.

Fractionating column item used in distillation of liquid mixtures

A fractionating column is an essential item used in distillation of liquid mixtures so as to separate the mixture into its component parts, or fractions, based on the differences in volatilities. Fractionating columns are used in small scale laboratory distillations as well as for large scale industrial distillations.

Gas chromatography common type of chromatography

Gas chromatography (GC) is a common type of chromatography used in analytical chemistry for separating and analyzing compounds that can be vaporized without decomposition. Typical uses of GC include testing the purity of a particular substance, or separating the different components of a mixture. In some situations, GC may help in identifying a compound. In preparative chromatography, GC can be used to prepare pure compounds from a mixture.

Forensic chemistry

Forensic chemistry is the application of chemistry and its subfield, forensic toxicology, in a legal setting. A forensic chemist can assist in the identification of unknown materials found at a crime scene. Specialists in this field have a wide array of methods and instruments to help identify unknown substances. These include high-performance liquid chromatography, gas chromatography-mass spectrometry, atomic absorption spectroscopy, Fourier transform infrared spectroscopy, and thin layer chromatography. The range of different methods is important due to the destructive nature of some instruments and the number of possible unknown substances that can be found at a scene. Forensic chemists prefer using nondestructive methods first, to preserve evidence and to determine which destructive methods will produce the best results.

Liquid chromatography–mass spectrometry

Liquid chromatography–mass spectrometry (LC-MS) is an analytical chemistry technique that combines the physical separation capabilities of liquid chromatography with the mass analysis capabilities of mass spectrometry (MS). Coupled chromatography - MS systems are popular in chemical analysis because the individual capabilities of each technique are enhanced synergistically. While liquid chromatography separates mixtures with multiple components, mass spectrometry provides structural identity of the individual components with high molecular specificity and detection sensitivity. This tandem technique can be used to analyze biochemical, organic, and inorganic compounds commonly found in complex samples of environmental and biological origin. Therefore, LC-MS may be applied in a wide range of sectors including biotechnology, environment monitoring, food processing, and pharmaceutical, agrochemical, and cosmetic industries.

Thickening agent substance used to increase viscosity of a liquid

A thickening agent or thickener is a substance which can increase the viscosity of a liquid without substantially changing its other properties. Edible thickeners are commonly used to thicken sauces, soups, and puddings without altering their taste; thickeners are also used in paints, inks, explosives, and cosmetics.

Solid phase extraction sample preparation process by which compounds that are dissolved or suspended in a liquid mixture are separated from other compounds in the mixture according to their physical and chemical properties

Solid-phase extraction (SPE) is a sample preparation process by which compounds that are dissolved or suspended in a liquid mixture are separated from other compounds in the mixture according to their physical and chemical properties. Analytical laboratories use solid phase extraction to concentrate and purify samples for analysis. Solid phase extraction can be used to isolate analytes of interest from a wide variety of matrices, including urine, blood, water, beverages, soil, and animal tissue.

Continuous distillation

Continuous distillation, a form of distillation, is an ongoing separation in which a mixture is continuously fed into the process and separated fractions are removed continuously as output streams. Distillation is the separation or partial separation of a liquid feed mixture into components or fractions by selective boiling and condensation. The process produces at least two output fractions. These fractions include at least one volatile distillate fraction, which has boiled and been separately captured as a vapor condensed to a liquid, and practically always a bottoms fraction, which is the least volatile residue that has not been separately captured as a condensed vapor.

Downstream processing refers to the recovery and the purification of biosynthetic products, particularly pharmaceuticals, from natural sources such as animal or plant tissue or fermentation broth, including the recycling of salvageable components and the proper treatment and disposal of waste. It is an essential step in the manufacture of pharmaceuticals such as antibiotics, hormones, antibodies and vaccines; antibodies and enzymes used in diagnostics; industrial enzymes; and natural fragrance and flavor compounds. Downstream processing is usually considered a specialized field in biochemical engineering, itself a specialization within chemical engineering, though many of the key technologies were developed by chemists and biologists for laboratory-scale separation of biological products.

Countercurrent distribution is an analytical chemistry technique which was developed by Lyman C. Craig in the 1940s. Countercurrent distribution is a separation process that is founded on the principles of liquid–liquid extraction where a chemical compound is distributed (partitioned) between two immiscible liquid phases according to its relative solubility in the two phases. The simplest form of liquid-liquid extraction is the partitioning of a mixture of compounds between two immiscible liquid phases in a separatory funnel. This occurs in five steps: 1) preparation of the separatory funnel with the two phase solvent system, 2) introduction of the compound mixture into the separatory funnel, 3) vigorous shaking of the separatory funnel to mix the two layers and allow for mass transfer of compounds in and out of the phases, 4) The contents of the separatory funnel are allowed to settle back into two distinct phases and 5) the two phases are separated from each other by draining out the bottom phase. If a compound is insoluble in the lower phase it will distribute into the upper phase and stay in the separatory funnel. If a compound is insoluble in the upper phase it will distribute into the lower phase and be removed from the separatory funnel. If the mixture contains one or more compounds that are soluble in the upper phase and one or more compounds that are soluble in the lower phase, then an extraction has occurred. Often, an individual compound is soluble to a certain extent in both phases and the extraction is, therefore, incomplete. The relative solubility of a compound in two phases is known as the partition coefficient.

Curing is a chemical process employed in polymer chemistry and process engineering that produces the toughening or hardening of a polymer material by cross-linking of polymer chains. Even if it is strongly associated with the production of thermosetting polymers, the term curing can be used for all the processes where starting from a liquid solution, a solid product is obtained.

A separation process is a method that converts a mixture or solution of chemical substances into two or more distinct product mixtures. At least one of results of the separation is enriched in one or more of the source mixture's constituents. In some cases, a separation may fully divide the mixture into pure constituents. Separations exploit differences in chemical properties or physical properties between the constituents of a mixture.

References

  1. ↑ J. W. Gooch, Analysis and deformulation of polymeric materials: paints, plastics, adhesives, and inks, Springer, May 31, 1997.
  2. ↑ S. Narayan, S. Thanedar, Overview of polymeric materials deformulation (1996) Technical Papers, Regional Technical Conference - Society of Plastics Engineers, pp. 125-128.
  3. ↑ M. L. Bruck, G. F. Willard, The Art and Science of Paint Deformulation, Metal Finishing, 104 (9), pp. 23-24.
  4. ↑ W. Hea, G. Cheng, F. Zao, Y. Lin, J. Huang, R. Shanks, Spectrochimica Acta Part A, 61 (2005) 1965–1970.
  5. ↑ Eldad Eilam, Reversing: Secrets of Reverse Engineering, Wiley, Indianapolis, 2005
  6. ↑ Andrew Huang, Hacking the Xbox: An Introduction to Reverse Engineering, Xenatera, 2003
  7. ↑ R. Chen, A. M. Tseng, M. Uhing, L. Li, J Am Soc Mass Spectrom 12 (2001)55–60.
  8. ↑ Craig L. Uhrich, The Economic Espionage Act—Reverse Engineering and the Intellectual Property Public Policy,7 Mich. Telecomm. Tech. L. Rev. 147 2001.
  9. ↑ P. Samuelson, S. Scotchmer, The Law and Economics of Reverse Engineering, The Yale Law Journal, 111, 1575-1663 April 10, 2002.
  10. ↑ J. C. J. Bart, Additives In Polymers: Industrial Analysis And Applications, Appendix II, John Wiley & Sons Ltd, 2005.
  11. ↑ H. Waldhoff (Ed.), R. Spilker (Ed.), Handbook Of Detergents Part C: Analysis, Marcel Dekker, 2005
  12. ↑ R. H. Leach, C. Armstrong, J. F. Brown, M. J. MacKenzie, L. Randall, H. G. Smith, The Printing Ink Manual 4th ed.,Blueprint, 1988, pp. 308-361.
  13. ↑ T. Kondo, E. Kanada, U. S. Patent 7,732,616, Lithographic Ink Additives.
  14. ↑ T. J. S. Learner, Analysis of Modern Paints, Getty Publications, 2004, pp. 20-29.
  15. ↑ E. Jablonski, T. Learner, J. Hayes, M. Golden, Conservation Concerns for Acrylic Emulsion Paints: A Literature Review,Tate's Online Research Journal. August 2004, Issue 2.
  16. ↑ E. E. K. Eisenhart, B. A. Jacobs, L. C. Graziano, U. S. Patent 6,180,242, Laminating Adhesive Composition, John Wiley and Sons, 2005.
  17. ↑ R. F. Haycock, A. J. Caines, J. E. Hillier, Automotive lubricants Reference Book, second edition,.
  18. ↑ P .L. K. Hung, M. L. Lavach. U. S. Patent 4,614,704, Stable UV curable compositions comprising triphenyl phosphite for forming solder mask coatings of high cure depth.
  19. ↑ D. P. Steen, P. R. Ashurst, Carbonated Soft Drinks: Formulation and Manufacture, Blackwell Publishing, 2006.
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