Applications

Near-Infrared spectroscopy (NIRS) is a widely used analytical technique for quantitative analysis of various products in research and industrial applications. This white paper summarizes the workflow of the development of quantitative methods according to ASTM E1655.

The acid number (AN) is a measure for the quality of oils and their potential to enhance corrosion. When analyzing fresh, unused oils, the AN is used to ensure the specified quality from the manufacturer, whereas for used oils the AN is determined to observe its increase until a critical level is reached. Although it is generally assumed that the AN correlates to the corrosive potential of the oil, this is not exactly correct, as it is the change of the AN value which indicates this issue. Therefore it is necessary to determine the AN on a regular basis.Several standards already exist to determine AN via titration methods, however it is also possible to measure this parameter via spectroscopic (NIRS) methodology. No matter which technique you choose, Metrohm has you covered with high-performance instruments suitable for these published norms.

More strict regulations paired with more complex products have increased testing complexity in the paint and coating industry. Therefore, producers ask for more powerful, safe and sustainable analytical methods. Testing by Vis-NIR spectroscopy is a sustainable and costefficient alternative to many wet chemical methods. This white paper describes how Vis-NIR spectroscopy improves testing procedures for various analyses during the formulation and production of paint and coatings in an economic and ecological way.Key words: testing, sustainable, VOC, paint, coating, binders, resins, additives, pigments, solvents

Printable Surface Enhanced Raman Scattering (P-SERS) silver substrates were used with Metrohm Raman’s Mira DS handheld Raman analyzer to successfully detect heroin in 18 crude street heroin samples. Detection of heroin with P-SERS was accomplished easily and very quickly, with minimal sample clean-up. Solvent studies were also implemented to determine the optimal solvent for crude sample extraction, with results included here.

Norms and Standards 21 CFR Part 11 is the FDA rule relating to the use of electronic records and electronic signatures.Recognizing the increasing impact of electronic media on critical data in regulated environments, the FDA met with members of the pharmaceutical industry in the early 1990s. The pharmaceutical industry and the FDA were interested in how they could accommodate paperless record systems and ensure the reliability, trustworthiness, and integrity of electronic records.

Data Integrity is currently a hot topic issue that has created much attention and has raised concern within companies working in regulated environments. This White Paper explains some of the key terms used in the context of Data Integrity and outlines how the requirements of Data Integrity can be understood and implemented.

Propylene oxide (PO) is a major industrial product used in assorted industrial applications, mainly for the production of polyols (the building blocks for polyurethane plastics). Several production methods exist, with and without co-products. This white paper lays out opportunities to optimize PO production for safer and more efficient processes, higher quality products, and substantial time savings by using online process analysis instead of laboratory measurements.

This Metrohm White Paper shows the requirements demanded of the pharmaceutical industry by the FDA with respect to software products. Implementation examples of the regulations formulated by the FDA in 21 CFR Part 11 are presented using Vision Air Pharma Software.Key words: electronic signatures, audit trails, user management, documentation

An analytic chemist in your back pocket. A forensic laboratory in a suitcase. A HazMat team in the trunk of your car. First responders need all the help they can get when faced with potentially dangerous substances. Mira DS from Metrohm Raman is a sophisticated chemical analyzer that replaces the specialist with automation. The push of a button initiates proprietary Smart Acquire routines to optimize acquisition parameters and collect the highest quality spectra. These spectra are automatically subjected to library search and Mixture Matching routines capable of identifying up to three components of a mixture. When hazardous substances are detected, the user is alerted to immediate action with color-coded warnings.

Chemometrics is a powerful tool widely used for method development in the pharmaceutical industry. This whitepaper describes the lifecycle of multivariate models and summarizes the workflow of the development of chemometrical models according to the new USP chapter <1039>.

Analytical Instrument Qualification (AIQ) according to the United States Pharmacopeia (USP) ensures that instruments perform as intended and users may have confidence in data quality. As the Pharma industry adopts handheld Raman instruments for incoming materials identification and verification, producers of such systems must provide suitable calibration and validation routines. Upon completion of these tests, end users are assured that all measurements are in accordance with agreed standards at Metrohm Raman, we have sophisticated AIQ routines in place to confirm the quality of your results.

This white paper differentiates between methods for identification of unknowns and verification of known materials. The goal of this publication is, ultimately, to inform the user of the capabilities of the handheld Metrohm Raman Mira P system. Best practices for building robust training sets for materials verification with Mira P can also be found here.

White paper about Raman spectroscopy and electrochemistry and their combination (electrochemical Raman).

The NanoRam is a state-of-the-art, handheld Raman spectrometer for the rapid identification of chemicals used in the pharmaceutical manufacturing process. It has been specifically designed for these applications and is fully compliant with all the major global regulatory, safety, and commercial testing agencies applicable to the pharmaceutical industry.

Raman spectroscopy is used widely by law enforcement as a field screening tool due to its speed, selectivity and ease of use. The majority of materials can be identified by the Raman signature, as they exhibit sharp distinctive peaks serving as a molecular fingerprint. However, many street and real-world samples are dark in color and not pure. The dark color, often due to impurities, gives rise to fluorescence that interferes with the Raman measurement. One method to suppress the fluorescence of a sample and enhance the Raman activity / signal is by the use of Surface-Enhanced Raman Spectroscopy (SERS).

Raman spectroscopy is an advantageous analytical tool that allows for the measurement of molecular structure and identifying chemical composition of materials based on the rotational and vibrational modes of a molecule. With advanced technology and an optimized optical design, the B&W Tek BAC102 series E-grade probe can access lower frequency modes down to 65 cm-1, providing key information for applications in protein characterization, polymorph detection, and identification, along with material phase and structure determination.

At a crime scene, a police officer collects a fiber sample that may prove to be invaluable evidence in identifying a criminal or exonerating an innocent person. In recent years, Raman spectroscopy has been studied extensively for forensic fiber analysis because of the high selectivity of Raman signatures, non-destruction nature of the test, and the ability to conduct the analysis without any sample preparation. The Raman spectrum can be measured directly on fabrics or fibers mounted on glass slide with very little interference from the mounting resin or the glass.

The benefits of a TE-cooled spectrometer in Raman systems are discussed to deliver lower system noise over longer integration times, resulting in lower limits of detection.

Conventional Raman typically has a very small sampling area with a high power density (PD) at the laser focal point on the sample, which means that only a limited portion of a sample is measured, and the result tends to be irreproducible for heterogeneous sample. The high power density may also cause samples to heat up or burn. The large spot adaptor (LSA) for B&W Tek’s handheld Raman products, featuring a much larger sampling area of 4.5 mm in diameter, is designed to overcome these issues.

The raw materials whey, sorbitol, stearic acid, and calcium phosphate dihydrate dibasic all show very distinctive, unique Raman signatures, which indicates that Raman spectroscopy is the ideal technology for identification of these materials. The PCA model-based method provides reliable specificity to successfully identify these nondestructively in plastc samples bags using the NanoRam.

Allowing non-destructive chemical identification through opaque materials, award-winning STRam represents an evolution in Raman technology.

Raman spectroscopy is a valuable tool to provide rapid, specific analysis for identification of raw materials, thus reducing the risk of using substandard or incorrect materials in manufacturing. The utility of handheld Raman increases productivity, and the ability to do full testing without creating bottlenecks in the production process. The integration of the Raman data into a company’s data management system provides a secure means of handling data and results, with reduced risk of transcription errors, and data loss.

Raman spectroscopy is used for material characterization by analyzing molecular or crystal symmetrical vibrations and rotations that are excited by a laser, and exhibit vibrations specific to the molecular bonds and crystal arrangements in the molecules. Raman technology is a valuable tool in distinguishing different polymorphs. Examples of portable Raman spectroscopy for identification of polymorphs and in monitoring the polymorphic transiton of citric acid and its hydrated form are presented.

This article demonstrates the utility of portable Raman spectroscopy as a versatile tool for process analytical technology (PAT) for raw material identification, in-situ monitoring of reactions in developing active pharmaceutical ingredients (APIs), and for real-time process monitoring. Raw material identification is done for verification of starting materials as required by PIC/S and cGMP, and can be readily done with handheld Raman. Portable Raman systems allow users to make measurements to bring process understanding and also provide proof of concept for the Raman measurements to be implemented in pilot plants or large-scale production sites. For known reactions which are repetitively performed or for continuous online process monitoring of reactions, Raman provides a convenient solution for process understanding and the basis for process control.

The suitability and potential of Raman spectroscopy in forensics is widely known by forensic specialists who use it in the laboratory to identify a wide variety of compounds including explosives, drugs, paints, textile fibers and inks. However, the use of laboratory-grade Raman outside the laboratory, such as for in‐situ analysis at a crime scene, was something thought possible only in forensic‐fiction until just a few years ago. Fortunately, modern portable Raman spectrometers are commercially available, and their instrumental features are comparable to Raman lab‐ spectrometers.To prove this, some extraordinarily demanding and challenging applications, in which an in‐situ standoff identification of samples might be advisable, were tested.

Forensics testing of samples encountered by law enforcement and customs agents is based on analytical techniques that are now being miniaturized and simplified and are making their way into field instrumentation. Field testing with Raman spectroscopy allows users to conduct reliable measurements at the point of arrest, reducing the burden on crime labs and accelerating the prosecution process.

Ternary mixtures of aqueous sugar solutions are measured and multivariate models of the concentration of analytes developed using BWIQ software.

Fiber-optic cables are marvels of innovation for modern spectroscopic instrumentation. The advantages offered by fiber optical cable-based sampling include great flexibility for enabling measurements at various sample sites, ease of use, and flexibility for easy transportation. With this freedom however comes increased responsibility for care and maintenance of the associated fiber accessories to ensure the measurement quality and fiber durability.

In this case study, a suspected counterfeit Adderall pill was measured directly with a TacticID Mobile using a point-and-shoot adapter. The spectra of the suspected couterfeit pill was found to contain cellulose and caffeine, but not the active ingredient. The TacticiD Mobile with 1064-nm laser excitation provides fluorescence suppression, giving those on the front lines a tool in the fight against dangerous counterfeit drugs.

Quantitation of the functionalization of a water-soluble polymer was achieved using a portable Raman spectrometer. The Raman spectrum provides strong, unique bands for both the initial and fully reacted polymer. This enables development of a simple, robust quantitative analysis of the percent polymer functionalization. This method is now routinely used in a manufacturing plant's quality control laboratory.

Raman spectroscopy is a valuable tool for the characterization of carbon nanomaterials due to its selectivity, speed, and ability to measure samples nondestructively. Carbon materials typically have simple Raman spectra, but they contain a wealth of information about internal microcrystalline structures in peak position, shape, and relative intensity.

This Application Bulletin compares the unique focusing technology of the portable Metrohm Raman system "Mira" with conventional methods. The method described here is called Orbital Raster Scan (ORS). Experiments show the advantages of ORS technology, using determination and quantification of medicines as an example. It improves the reproducibility of the Raman signals from targeted, active, pharmaceutical ingredients (APIs) in effervescent, cold medicines. Shorter analysis times and an improved, consistent assignment of spectra of the known medicine with the help of a spectral library are further advantages of ORS technology.

The present Application Bulletin contains NIR applications and feasibility studies using NIRSystems devices in the pharmaceutical industry. Qualitative and quantitative analyses of a wide variety of samples are part of this bulletin. Each application describes the instrument that was originally used for the analysis, as well as the system recommended for the analysis and the results that were achieved thereby.

The present Application Bulletin contains NIR applications for the determination of important parameters for pulp and paper quality analysis. Each application describes the instrument that was originally used for the analysis, as well as the system recommended for the analysis and the results that were achieved thereby.

This Application Note shows that NIR spectroscopy is an excellent tool for determining low concentrations of additives in finished polypropylene pellets. This is demonstrated by monitoring the UV stabilizer Tinuvin 770 and the antioxidant Irganox 225. The application of multiple linear regression (MLR) models minimizes interferences that originate from different coating thicknesses and interferences in the polymer pellets.

Near-infrared spectroscopy (NIRS) is ideally suited to monitor the hardwood and softwood content in pulp and paper products.The herein described method bases on the fact that the changes in hardwood and softwood content are reflected in the intensity of the absorption bands of cellulose. A linear least-squares regression on second derivative spectra provide results that correspond very well with those of conventional laboratory determinations. With NIRS, an analytic method is available that provides results in real time.

This Application Note shows the fast and parallel determination of water content and pH value in crude tall oil samples using near-infrared spectroscopy (NIRS). Crude tall oil is an important byproduct of pulp production in the power process. NIRS is an efficient alternative to conventional laboratory methods: It permits rapid raw material inspection, process monitoring and final product checking.

Visible Near-infrared (Vis-NIR) spectroscopy is a valuable chemical analysis tool that can be used to determine quality parameters of hair creams. A qualitative method was developed in order to allow a fast out-of-spec analyses of an active antibacterial ingredient.

Near-infrared spectroscopy (NIRS) was used as an analysis method for quality control of soap noodles. Quantitative models for the determination of Total Fatty Matter, Iodine Number, and C8–C14 were developed, enabling fast and reliable quality control.

Near-infrared spectroscopy (NIRS) was used for quality control of skin creams. A model for the quantification of the water content was developed based on Karl Fischer titration (KF), enabling fast and reliable atline analysis and final product quality control.

This Application Note describes a fast method for the simultaneous quantification of nicotine and glycerin in liquid mixtures used for electronic cigarettes. With visible near infrared spectroscopy (VIS-NIRS), results are available without sample preparation, thus making VIS-NIRS highly suited for fast quality control.

Packaging has become an indispensable part in the food manufacturing process. To improve the appearance and properties of the packaging, a wide variety of coatings and inks are used. Different additives enhance rheological properties, control the wetting dispersion, or in the case of wax increase abrasion resistance. The regulations of these coatings in food packaging applications are very strict in some countries, creating the need for close monitoring of the production process.A fast, reliable, and simple to use solution for quantifying rheological additives and wax in such coatings is Visible-Near Infrared Spectroscopy (Vis-NIRS). Both parameters are determined simultaneously by Vis-NIRS in less than a minute.

This Application Note describes an NIR method for monitoring the esterification process in butyl acetate production. The developed NIR method shows excellent analytical performance equivalent to that obtainable with more time-consuming GC methods.

Well-mixed active substances for medications are indispensable in the pharmaceutical industry. This applies not only to the pharmaceutical active ingredient but also for lubricants, binding agents, explosives, oxidants and dyes. Analysis of these active ingredients is expensive; they are also only rarely analyzed as a rule. The progress of the mixing procedures can be followed conveniently with NIR spectroscopy, on the one hand using visual comparisons and on the other by means of spectral algorithms. The progress of mixing processes can be predicted in real time with the help of the spectrum when the latter is used.

This Application Note shows how, with the help of Vis-NIR spectroscopy and a special plant library, 46 different medicinal and aromatic plants, e.g., Organicum majoricum and Tilia cordata, can be conveniently identified on the basis of their spectrum. In comparison with alternative methods for the determination of plants, which are elaborate and require experienced scientists for their performance, the Vis-NIR method permits rapid and uncomplicated identification.

This Application Note shows how purity, degree of substitution and water content of carboxymethyl celluloses (CMC) can be determined conveniently and rapidly in a single measurement with Vis-NIR spectroscopy.

This Application Note demonstrates the data transfer from a Fourier transform to a dispersive NIR instrument, using quality control of lubricating oils as an example application. It is shown that FT-NIR instruments can be replaced by dispersive ones without time-consuming sample remeasurement and subsequent method development.

Near-infrared spectroscopy (NIRS) was used as an analysis method for quality control of aqueous xanthan gum solutions. Quantitative models for the determination of optical density, glucose, and xanthan gum were developed, enabling fast and reliable quality control.

This Application Note describes the determination of multiple quality parameters (hydroxyl number, acid number, and moisture content) of polyols using Vis-NIRS. Without any sample preparation, this unique analytical technique enables straightforward quantitative analysis.

This Application Note describes the simultaneous determination of the four most important analysis parameters of paint dryers – cobalt and solids contents, specific weight and viscosity – using a VIS-NIR analyzer. The visible range correlates with the metal content, while the NIR region provides the specific weight, viscosity and solids content.