Applications

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).

The emergence of counterfeit prescription drugs has become a concern for the pharmaceutical industry. Because of the low concentrations of APIs found in pharmaceutical drugs, normal Raman spectroscopy is typically not sensitive enough to detect the API from the surface of a pill. In this study we develop a surface-enhanced Raman spectroscopy (SERS)-based approach to identify a low-dose of the API alprazolam in a Xanax tablet using a handheld Raman spectrometer. If no SERS peaks consistent with alprazolam are observed from a Xanax tablet, the pill is a suspected fake. The method demonstrates the power of SERS to quickly verify the presence of alprazolam in the tablet for anti-counterfeiting purposes.

A new Raman system design is presented that expands the applicability of Raman to See Through diffusely scattering media such as opaque packaging materials, as well as to measure the Raman spectrum and identify thermolabile, photolabile, or heterogeneous samples.

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.

Law enforcement personnel, laboratory technicians, crime scene investigators and many others face a significant challenge for identification of materials in a forensic investigation.Traditionally, technicians used multiple forms of identification in order to collect results from various forms of forensic samples. Although certain technologies are ideal for precise laboratory identification, many technologies, such as Raman spectroscopy, can be successfully used for identification of multiple forensic sample types either directly in the field or in the lab. Raman spectroscopy is classified as a Category A analytical method by the Scientific Working Group for the Analysis of Seized Drugs (SWGDRUG; Version 7.1, 2016).

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.

B&W Tek’s TacticID®-1064 is a field-ready handheld Raman system utilizing 1064-nm wavelength laser excitation. Designed for forensic analysis by safety personnel, first responders, and law enforcement personnel, the TacticID-1064 significantly reduces fluorescence, allowing users to identify tough street samples such as ecstasy tablets in a variety of colors and mixture forms.

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.

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 TacticID®-1064 ST is a 1064 nm handheld Raman system designed for law enforcement officials, first responders, and customs and border protection officers for rapid field identification of illicit substances such as narcotics, explosives, and other suspicious materials.The TacticID-1064 ST is specially designed with see-through Raman functionality to measure materials through both transparent and opaque containers. These through-barrier measurements remove the need for active sampling of potentially dangerous compounds such as fentanyl, leading to safer operations and reduced wait time for clear results.

Although the process of building, validating and using a method is well-defined through software, the robustness of the method is dependent on proper practice of sampling, validation, and method maintenance. In this document, we will detail the recommended practices for using the multivariate method with NanoRam-1064. These practices are recommended for end users who are in the pharmaceutical environment, and can expand to other industries as well. This document aims to serve as a general reference for NanoRam-1064 users who would like to build an SOP for method development, validation and implementation.

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.

Psychoactive gamma-hydroxybutyrate (GHB) and its prodrug gamma-butyrolactone (GBL) are substances that are increasingly abused as date-rape and recreational (party) drugs. Since the non-controlled GBL converts into the illicit GHB both in-vivo and in-vitro, their legal distinction is of crucial importance.For the forensic determination of illegally added GHB and GBL in commonly consumed beverages, this work presents a simple and sensitive method that employs direct-injection ion chromatography combined with spectrophotometric detection. The method allows to trace GHB-GLB interconversion, whether in vivo or in vitro lactone cleavage or intramolecular GHB esterification, and thus complies with pertinent requirements of law enforcement agencies.

Determination of chlorine in household bleaches.

Fentanyl, a powerful synthetic opioid, is illegally distributed worldwide. Overdosing can be fatal, causing symptoms like stupor, pupil changes, cyanosis, and respiratory failure. Just 2 mg of fentanyl can be lethal, depending on factors like body size and past usage. Given its severe impact, identifying and detecting fentanyl is crucial, as it has become a major public health crisis. Combining electrochemical surface-enhanced Raman spectroscopy (EC-SERS) with screen-printed electrodes (SPEs) offers a fast, effective, and precise method for detecting fentanyl.

Acid throwing, a historical method for retribution against women, has become a modern threat of a different nature. Concentrated acids and other corrosive substances have emerged as modern tools of social violence. Aggressors use common plastic containers with openings that create a powerful directional spray, such as lemon juice squeeze bottles. Sulfuric and phosphoric acids were chosen for analysis here due to their highly corrosive nature- acid attacks in London most commonly use sulfuric, phosphoric, and nitric acids.2017 saw a remarkable number of acid attacks in the UK, with reported incidences averaging 2x a day. Detection and regulation of acids may contribute to prevention of this social scourge.

Identification of unknown materials in the field can be a complicated affair, especially in critical situations, where speed, safety, and ease-of-operation are essential. Mira DS, Metrohm Raman’s handheld Raman analyzer, and the intelligent Universal Attachment (iUA) give the user automated Content ID capabilities. Content ID achieves through container identification of unknown materials quickly, easily, and safely.

Handheld Raman spectrometers are valued for their ability to provide onsite material identification in seconds. In the case of combination pharmaceuticals, a single tablet contains more than one active ingredient in different proportions. MIRA DS is uniquely capable of identifying multiple compounds in such tablets by using Raman to identify the major component and SERS (surface-enhanced Raman spectroscopy) for the minor component. This application describes quick, dual analysis of a prescription medication containing acetaminophen and hydrocodone. The application is easily extrapolated to the study of street drugs.

Yaba, produced in Southeast Asia, is a popular drug of abuse and is actively targeted by police squads. Two strong and highly addictive stimulants make up Yaba: caffeine, which comprises up to 60% of each tablet, and methamphetamine at approximately 20%. Identifying these two active ingredients in different proportions in a colorful tablet with other excipients could be an analytical nightmare. With handheld Raman, bulk material identification is achieved in seconds onsite with simple point-and-shoot analysis. SERS (surface-enhanced Raman spectroscopy) analysis is used to detect the minor component in mixtures without interference from fillers, dyes, and coatings. MIRA DS is uniquely capable of both analyses—Raman testing positively identifies caffeine in Yaba, while methamphetamine can be detected with SERS sampling. This application describes quick, dual analysis of Yaba tablets with MIRA DS.

Raman analysis of fentanyl-soaked paper, SERS detection range for fentanyl on paper, and real-world example of fentanyl identification.

Signal-to-noise ratio, spectrograph design, resolution of MIRA handheld Raman analyzers.

With MISA and MIRA, easy-to-use test kits and flexible sampling allow rapid and accurate interrogation of suspect materials with minimal time, training, and expense.

TacticID-1064 ST is a handheld Raman device that can identify materials through paper, plastic, glass, and multilayer packaging, reducing exposure risks and eliminating the need to open containers.

Determination of chlorate, nitrate, and perchlorate in firecracker powder using anion chromatography with conductivity detection after chemical suppression.

Determination of chloride, nitrite, cyanate, azide, nitrate, chlorate, sulfate, thiocyanate, thiosulfate, and perchlorate in an extract of explosives using anion chromatography with conductivity detection after chemical suppression.

The Dose-in Gradient expands the standard IC system to a gradient system. Using isocratic elution for separating the oxyhalides and the anions containing sulfur is very time-consuming. An 800 Dosino and a T-piece are used to expand the isocratic system to a binary gradient system. This is shown in the example of the determination of the standard anions, in addition to chlorate, thiosulfate, thiocyanate, and perchlorate.

4-Hydroxybutyrate (GHB) is numbered among the hydroxycarboxylic acids and is used as a psychoactive drug which is illegal in many countries. GHB can be determined through anion chromatography with suppression. GHB can be separated from the standard anions and the organic acid anions glycolate, acetate and formate on the Metrosep A Supp 16 - 250/4.0 column and under the conditions specific in this Application Note.Key words: Liquid Ecstasy, KO drops

Forensic institutes examine terrorist attacks and warfare agents via trace detection analysis of the used explosives and their residuals. Of particular importance is the acquisition of «chemical fingerprints» for criminal investigation departments and governmental security agencies. Institutes for public health and environmental protection analyze such compounds that can contaminate the underlying soil and infiltrate ground water.Forensic investigation with ion chromatography (IC) using suppressed conductivity detection allows a sensitive and robust determination of anionic contaminants such as chlorate, thiosulfate, thiocyanate, and perchlorate next to the common inorganic anions over a broad concentration range.

Peroxides are often used for disinfection and water treatment purposes due to their antiseptic properties. Lower concentrations between 0.3–3% are used in households, while higher concentrations can be used for sterilization purposes. Additionally, peroxides are utilized as oxidizing and bleaching agents. Peroxides, perborates, and percarbonates can easily be determined by titration. This application note presents two titration methods for peroxide analysis: ASTM D2180 for concentrated hydrogen peroxide solutions, and a second method for trace determination of hydrogen peroxide, suitable for concentrations as low as 0.4 mg/L.

Today's Raman instrumentation is faster, more rugged, and less expensive than in the past and the advances in component miniaturization have led to the design of portable devices with extremely high performance designed for field-based investigations. This study focuses on the use of handheld Raman spectroscopy for the characterization and identification of samples encountered in various application areas related to forensic science.

Small, fast high-performance Raman spectrometers are now readily available. Three real-life Raman quantitative and semi-quantitative analysis applications are discussed. These applications showcase the versatility of Raman spectroscopy and the potential impact that it can make in various industries such as security, pharmaceutical, and plastics and polymers.

Patented STRaman technology is a new Raman technique that can identify chemical species nondestructively beneath diffusely scattering packaging material such as plastics or tablet coatings.

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

Surface Enhanced Raman Scattering or SERS is an anomalous enhancement of Raman scattering when molecules are adsorbed to gold or silver nanoparticles – this enhancement can be as large as 107. The advantage of SERS for the analytical chemist lies in its ability to detect analyte concentrations of parts per million and even parts per billion levels, while classical Raman is limited to parts per thousand. Metrohm Raman produces P-SERS assays in the form of nanoparticles printed onto substrates using inkjet technology. This method produces inexpensive test strips that exhibit exceptional stability and sensitivity. There are two markets that can be easily addressed with P-SERS: forensic analysisand food safety. This white paper explains the mechanism of SERS and how it can be applied to handheld Raman analysis with Metrohm Raman Mira systems.

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.

Metrohm Raman presents a unique handheld materials identification system designed to meet the needs of defense and security professionals. Meet Mira DS, the most adaptable Raman analyzer available today. Mira DS was developed directly in response to requests from first responders in the field for a small, rugged, automated materialsidentification system that ensures the safety of the user in any situation.

Detection of threatening materials requires robust and sophisticated instruments capable of safe, instantaneous field-analysis of unknowns. In an environment where there is an ever-evolving threat of explosives made from commonlyavailable chemicals, explosive libraries must be customized constantly to include newly targeted materials. Mira DS from Metrohm Raman is the perfect solution for detection of explosives in the field. This handheld Raman instrument is equipped with sophisticated analysis algorithms and a suite of safety features for first responders who need the identity of a potential hazard... NOW! Mira DS and its software can be customized to respond to emerging hazards: this note describes procedures for creating custom libraries of binary explosive precursors to be used in library comparison and mixture matching routines on Mira DS. With these tools, unknown substances can be identified with color-coded warnings for fast action in critical situations.

A person suspected of possessing a narcotic can be charged with a crime only after the identity of the illicit substanceis confirmed. This confirmation is typically provided by analytical chemists in forensic laboratories and requires highly technical separation and detection methods. Unfortunately, such labs often have deep caseloads that lead to delays in testing. Handheld Raman analyzers bring the reliability and accuracy of lab analysis to first responders in the field, allowing for rapid and accurate identification of street drugs with a white powder appearance. With such tools, demand for forensic analysis can be reduced and enforcement agencies can enforce drug policies with greater safety, speed, and precision.

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.

Like any defense and security professional, border agents must quickly and accurately identify suspicious substances at the point of contact. When that substance is fentanyl, which is deadly in microdoses, the stakes are even higher. The Mira DS handheld Raman system from Metrohm Raman offers safe, no-contact identification of over 200 fentanyl analogues. Mira DS protects border agents, while they protect citizens from deadly narcotics, drug smugglers, and illegal entry of goods.

In this White Paper, you will learn about MIRA XTR DS – the smallest, smartest, most flexible handheld Raman system with the largest libraries available on the market! MIRA XTR DS has all the benefits of 785 nm Raman interrogation: compact size, low laser power, sample preservation, long battery lifetimes... now with fluorescence rejection. Additionally, there is improved sensitivity and resolution over 1064 nm systems. This opens up new possibilities for 785 nm Raman, including strongly colored materials, common excipients, illicit materials, and more.

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