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Portable Raman spectroscopy is an invaluable tool in the study of archaeological sites, allowing for in situ analysis which minimizes the impact of such studies on important cultural sites. The flexibility of the use of a fiber optic probe and tripod-mounted video microscope with a light weight instrument reduces the need for sampling, and increases the ability to make representative measurements over what can be very large sample areas. The information content of Raman spectroscopy aids in the understanding of the materials used in the construction and restoration of important archaeological sites, and in understanding the degradation that is occurring which should aid in preservation and restoration work.

For SERS developers and end users of SERS for specific applications to investigate low concetation levels of compounds, the centerpiece of their technological platform must be a Raman setup that provides reliable lab grade performance and is affordable and portable, allowing them to tackle real world problems. The portable i-Raman Plus system coupled with a BAC151 video microscope sampling accessory provides an ideal setup. With the performance and flexibility of use with different laser spot size and power for SERS research.

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.

Portable Raman is used to quantify trigonelline, an alkaloid that contributes to the health benefits of some foods. A simple method to quantify the presence of diluted trigonelline in solutions using surface enhanced Raman spectroscopy is described. Portable Raman is a tool that could be used in quality control of food items such as coffee and quinoa.

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.

Correct identification of mineral phases in rock thin sections is essential to petrographic and petrologic analysis of rocks. Portable Raman coupled to an optical microscope gives chemical information along with the optical images to give a higher certainty of identification than traditionally used optical micropcopy alone.

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.

Raman spectroscopy’s use for process analytics in the pharmaceutical and chemical industries continues to grow due to its nondestructive measurements, fast analysis times, and ability to do both qualitative and quantitative analysis. Spectral preprocessing algorithms are routinely applied to quantitative spectroscopic data in order to enhance spectral features while minimizing variability unrelated to the analyte in question. In this technical note we discuss the main preprocessing options pertinent to Raman spectroscopy with real applications examples, and to review the algorithms available in B&W Tek and Metrohm software so that the reader becomes comfortable applying them to build Raman quantitative models.

This work was carried out with a Metrosep C 2 - 150 separation column, the following eluent parameters being investigated: nitric, tartaric, citric and oxalic acid concentration and concentration of the complexing anion of dipicolinic acid (DPA). The aim was to determine the effect of these parameters plus that of the column temperature on the retention times of alkali metals, alkaline earth metals, ammonium and amines using ion exchange chromatography with non-suppressed conductivity detection. Due to similar affinities for the ion exchange column, transition metals are difficult to separate with the classical nitric, tartaric, citric and oxalic acid eluents. Partial complexation with the dipicolinate ligand significantly shortens the retention times and improves the separation efficiency. However, too strong complexation results in a rapid passage through the column and thus in a complete loss of separation. Apart from a change in the elution order of magnesium and calcium at high DPA concentrations, other non-amine cations are only slightly affected by the eluent composition. Irrespective of the tartaric acid and nitric acid concentration in the eluent, an increase in column temperature shortens the retention times and slightly improves the peak symmetries of organic amine cations, particularly in the case of the trimethylamine cation. In contrast, an increase in column temperature in the presence of DPA concentrations exceeding 0.02 mmol/L increases the retention time of the transition metals. Depending on the separation problem, variation of the pH value, the use of a complexing agent and/or an increase in column temperature are powerful tools for broadening the scope of cation chromatography.

Metrohm's iColumns are the first IC columns that are equipped with a data chip that stores freely definable data, fixed column data as well as data entered by the MagIC NetTM software. Any relevant information such as column type, standard parameters, maximum pressure, etc. can be called up at any time. Analysis data continuously entered by the MagIC NetTM software guarantees a complete column and GLP-compliant surveillance irrespective of the IC system in which the column is operated. The MagIC NetTM software surveys the critical column data and indicates any infringement of limits.

By using the 800 Dosino and the 849 Level Control as the only additional devices, Metrohm`s intelligent ion chromatography (IC) systems - the 850 Professional IC and the Compact IC family - can be easily extended to perform any unattended inline eluent preparation. Fully controlled by MagIC NetTM, the 849 Level Control monitors the eluent level while the Dosino performs all dosing and liquid handling tasks. Consecutive injections of a 250-µg/L standard over approximately 20 days revealed an excellent retention-time stability. After more than 800 consecutive injections, relative standard deviations for anions (F-, Cl-, NO2-, Br-, NO3-, PO43-, SO42-) and cations (Li+ , Na+, NH4+, K+, Ca2+, Mg2+) were smaller than 0.55 and 0.41%, respectively. In the case of a 24-hour sequence, retention-time precision for anions and cations was better than 0.09 and 0.08%, respectively. The presented inline eluent preparation system increases the retention-time reproducibility and allows the determination of anions and cations over a one-month period without manual eluent preparation.

Comparative measurements show that the new Metrosep C 4 cation column has even better separation characteristics than the previous Metrosep C 2 and Metrosep Cation 1-2 column types. The Metrosep C 4 column has a clearly improved peak shape which leads to a better separation of the individual peaks. Using Metrosep C 4 the number of theoretical plates per meter was noticeably higher than that obtained on the Metrosep C 2 or C 1-2 column. Additionally for standard cations transition metals and amines, the Metrosep C 4 column shows better results with respect to peak shape, peak height, resolution and asymmetry factor. The clearly improved resolution of the C 4 column with its narrow and high peaks achieves baseline separation for six standard and six transition metal cations. Analysis times and peak areas obtained with the C 4 column are in the same range as those obtained with its predecessors.As a result of the latest production methods and materials, the promising Metrosep C 4 column excels by an outstanding separation performance for complex mixtures comprising standard cations, transition metal cations and amines.

The combination of 850 Professional IC, 858 Professional Sample Processor, Dosino and MagIC NetTM software offers a variety of automated ion chromatographic sample preparation and calibration techniques available as an anion, cation or dual channel system. Calibration is straightforward and requires only one multi-ion standard.Inline calibration allows the calibration of any standard concentration in the ppt range by using one single stable standard solution at the ppb level. By using a preconcentration column and switching the valves one, two or more times different calibration concentrations at the ultra-trace level can be created with unprecedented reproducibility. The inline preconcentration technique uses a pre-concentration column and is ideally suited for trace analysis in complex matrices, especially when combined with matrix elimination. Besides facilitating the preparation of g/L to ng/L calibration graphs Metrohm`s intelligent techniques are capable of logical decision making. While Metrohm`s intelligent Partial Loop technique (MiPT) allows samples with a wide concentration range to be injected without previous manual dilution, the intelligent inline dilution technique, after the first sample injection, compares peak areas, calculates, if necessary, the dilution factor, dilutes and automatically re-injects the sample. The presented inline techniques allow the rationalization of the time-consuming, error-prone and cost-intensive manual preparation of standard solutions. They guarantee that the determined sample concentrations always lie within the calibration range. Higher sample throughputs as well as lower analysis costs and improved data reliability are achieved.

Inline coupling of the 815 Robotic Soliprep with an ion chromatograph (IC) allows the straightforward determination of anions and cations in tablets. After automatic solvent addition and subsequent comminution, the homogenized tablet samples (Singulair and Bezafibrat) are filtered and subsequently transferred to the injector. The completely automated sample preparation saves both time and money, guarantees traceability of each sample preparation step and yields correct and precise results. In the range of 0.2…50 mg/L, six-point calibration curves for anions and cations yield correlation coefficients better than 0.99990 and 0.99991, respectively. While relative standard deviations (RSDs) for sub-ppm levels of nitrate, sulfate, calcium and magnesium in Singulair and Bezafibrat are smaller than 3.64%, RSD of ppm levels of chloride is better than 0.83%. The application of further inline sample preparation steps such as pulverizing, extracting, filtering or diluting facilitates numerous custom-tailored setups for ion determinations in exacting matrices such as animal feed, sediments or food.

In routine chemical analysis, the predominant challenge involves a higher sample throughput, improved reproducibility, liquid handling flexibility and reduced personnel costs. In response to these requirements, the 872 Extension Module Liquid Handling in combination with the MagIC NetTM software and the well-proven Dosino technology expands the possibilities of inline sample preparation and opens up new fields of application. Among others, the module can be used, together with an optional mixing vessel, for pH adjustments, pre-column derivatizations, or the mixing of solutions.As a representative of an inline sample preparation technique, this poster describes the performance of precise dilutions. By using only one single stable standard solution, multi-point calibration curves can be automatically recorded by diluting a concentrated standard in an external vessel.

Available sample size, mass sensitivity, efficiency and the detector type are important criteria in the selection of separation column dimensions. Compared to conventional 4 mm i.d. columns, microbore columns excel, above all, by their low eluent consumption. Once an eluent is prepared, it can be used for a long time. Additionally, the lower flow rates of microbore columns facilitate the hyphenation to mass spectrometers due to the improved ionization efficiency in the ion source.With the same injected sample amount, a halved column diameter involves a lower eluent flow and results in an approximate four-fold sensitivity increase. In a converse conclusion, this means that with less sample amount, microbore columns achieve the same chromatographic sensitivity and resolution than normal bore columns. This makes them ideally suited for samples of limited availability.

Metrohm`s intelligent Preconcentration Technique with Matrix Elimination (MiPCT-ME) excels in its capacity to perform automatic ion chromatographic determinations over 6 orders of magnitude. Crucial requirements for this are the system`s intelligence and the exact measurement of the sample volume. While the intelligence allows to compare results and take decisions, the dosing device takes over the high-precision liquid handling of even single-digit microliter volumes to the preconcentration column. By using only one analytical setup and without additional rinsing, samples containing both ultratraces and high concentrations can be analyzed.As the other Metrohm Inline Techniques, the MiPCT-ME technique presented reduces the workload, ensures complete traceability, is free of carryover effects and significantly improves accuracy and reproducibility of the results.

The poster describes how different suppressors (MSM and MCS) work and mentions possible applications.

By combining the information from electrochemical and spectroscopic techniques, UV/VIS spectroelectrochemistry (UV/VIS-SEC) allows a comprehensive analysis of electron-transfer processes and complex redox reactions. The anodic oxidation of a N-aryl-D2-pyrazoline derivative was investigated by combining cyclic voltammetry and UV/VIS spectroscopy. In-situ measured UV/VIS absorbance depicted the absorption changes that accompanied the anodic oxidation and could therewith prove the stability of the electrogenerated radical cation. UV/VIS-SEC provides a powerful tool for the in situ study of shorter-lived species, reaction mechanims, and kinetics in a wide variety of electrochemical active organic, inorganic, and biological molecules.

It is a comparatively easy matter to coat platinum electrodes with platinum black by electrolytic deposition of the metal from a platinizing solution.

This bulletin contains two parts. The first part gives a short theoretical overview while more details are offered in the Metrohm Monograph Conductometry. The second, practice-oriented part deals with the following subjects:Conductivity measurements in general; Determination of the cell constant; Determination of the temperature coefficient; Conductivity measurement in water samples; TDS – Total Dissolved Solids; Conductometric titrations;

In our Instructions for Use for the 656 Electrochemical Detector the user will find all the basic information about how it works and how to use it as well as how to handle the electrodes. They also contain information about the demands placed on the separating system together with the causes of and remedies for detection problems.Application Bulletin no. 128 is intended to provide an overview of the most important substance classes and mention some compounds that can easily be determined oxidatively, i.e., with detection limits in the pg range; it also mentions possible working conditions for separation and electrochemical detection and illustrates them with examples.

This Application Bulletin gives an overview of the coulometric water content determination according to Karl Fischer.Amongst others, it describes the handling of electrodes, samples, and water standards. The described procedures and parameters comply with the ASTM E1064.

This Bulletin, using practical examples, indicates how the user can achieve optimum pH measurements. As this Bulletin is intended for actual practice, the fundamentals - which can be found in numerous books and publications - are treated only briefly.

This Bulletin provides an overview of the potentiometric titer determination of current titrants. Many publications only describe methods with color indicators. However, the titration conditions chosen for the titer determination should resemble those used for the actual analysis as closely as possible. The tables contain suitable titrimetric standard substances and electrodes for selected titrants as well as additional information. Following this, an example is given to show what an SOP for a titer determination could look like.

The sample preparation for ion chromatography is divided into steps which should generally be implemented to preserve the column and into steps which should be performed to obtain an improved chromatogram. The goal is to have the test substance in ionic form in solution without the presence of interfering substances.

This Bulletin describes the determination by ion chromatography of anions, particularly fluoride, chloride, nitrite, bromide, nitrate, and sulfate using the Hamilton PRPX100 IC anion column without chemical suppression.

This Application Bulletin describes methods for checking the condition of electrodes for surfactant titration. For testing electrodes used for ionic surfactant titration (Ionic Surfactant electrodes), sodium dodecyl sulfate (SDS) is determined using TEGO®trant. Conversely, for testing electrodes used for cationic surfactant titration (Cationic Surfactant electrodes), TEGO®trant is titrated with SDS.For non-ionic surfactant electrodes (NIO surfactant electrode), PEG 1000 is titrated with sodium tetraphenylborate (STPB).For testing Surfactrode Resistant and Surfactrode Refill electrodes, titrations of SDS with TEGO®trant are performed. Suitable criteria for the test are the height of the potential jump and the shape of the titration curve.Key word: NaPh4B

Lithium-ion batteries must be completely free of water (concentration of H2O < 20 mg/kg), because water reacts with the conducting salt, e.g., LiPF6, to form hydrofluoric acid.The water content of several materials used in lithium ion batteries can be determined reliably and precisely by coulometric Karl-Fischer titration. In this Application Bulletin the determination for the following materials is described:raw materials for the manufacture of lithium-ion batteries (e.g., solvents for electrolytes, carbon black/graphite); electrode coating preparations (slurry) for anode and cathode coating; the coated anode and cathode foils as well as in separator foil and in the combined material; electrolytes for lithium-ion batteries;

Eco Titrators provide the capability to send PC/LIMS reports directly to a PC. This feature is mainly used to transfer data to an external LIMS system or to simply store the data in a digitally on the PC. Additionally, it is possible to control the Eco Titrator by RS232 commands if the connection is set up according to the procedure described below.The data transfer from the Eco Titrator to a PC can be done by a software- or a hardware-based option. Additional accessories are needed for the hardware-based option whereas for the software-based option two additional softwares must be installed. Both solutions are described in this document.

Automatic sample handling and analysis is very convenient for routine measurements on large number of samples. Metrohm offers a wide range of high performance liquid handling devices that can be combined with the Autolab product range and can be directly controlled by the NOVA software.

The Metrohm 800 Dosino is the workhorse of any automated liquid handling setup. This instrument can be conveniently used in combination with the NOVA software and integrated conveniently with electrochemical measurements performed with the Autolab systems.

The Metrohm 858 Professional Sample Processor is a robotic liquid handling system capable of handling large series of samples automatically. This instrument provides a platform that can be directly controlled by the NOVA software and combined with the Autolab potentiostat/galvanostat for automated high-throughput electrochemical measurements.

In this application note, we demonstrate how to determine the binary diffusion coefficient of a commercial liquid binary lithium ion battery electrolyte based on a galvanostatic pulse polarization method.

This application note presents the experimental details and an overview of the most important findings from the EIS and CV experiment to study the structure of a model solid electrolyte interface forming on a planar glassy carbon electrode in contact with a typical organic battery electrolyte.

In this application note, we demonstrate how to determine the through-plane tortuosity τ of a commercial lithium ion battery cathode material with known porosity and coating thickness, based on the electrochemical impedance spectroscopy (EIS) method.

In this application note, we demonstrate how to determine the lithium ion transference number of a commercial liquid binary lithium ion battery electrolyte, based on the very-low-frequency electrochemical impedance spectroscopy (VLF-EIS) method.

In battery research, electrochemical impedance spectroscopy (EIS) is a necessary tool to investigate the processes occurring at the electrodes. With a common three-electrode battery, EIS can be performed sequentially first at one electrode and then at the other electrode.

This Application Note explains how researchers can determine the underlying chemistry and potential failure mechanisms from cycle testing batteries with INTELLO.

This Application Note discusses differential capacity analysis (DCA) and its impact on enhancing battery performance, with a focus on using the INTELLO platform.

The use of an appropriate full scale together with the zero function of the 732 IC Detector minimizes baseline noise dramatically. Much lower detection limits are achieved.

Determination of aluminum using cation chromatography, post-column reaction and UV detection.

Determination of lead, zinc, indium, cadmium, cobalt, ammonium, potassium, manganese, magnesium, and calcium using cation chromatography with direct conductivity detection.

Determination of mono-, di-, and trimethanolamine (MMA, DMA, TMA respectively), in the presence of lithium, sodium, ammonium, potassium, magnesium, cesium, calcium, and strontium using cation chromatography with direct conductivity detection.

Determination of traces of methylamine, isopropylamine diethylethanolamine, and diethylamine in the presence of lithium, sodium, ammonium, potassium, magnesium, and calcium using cation chromatography with direct conductivity detection.

Determination of traces of ammonium in the presence of sodium, potassium, magnesium, and calcium using cation chromatography with direct conductivity detection.

Determination of traces of lutetium, ytterbium, thulium, erbium, terbium, gadolinium, samarium, neodymium, praseodymium, cerium, and lanthanum using cation chromatography with gradient elution and UV/VIS detection after post-column reaction with Arsenazo III.

Determination of hydroxylamine, ethanolamine, triethanolamine, and hydrazine using cation chromatography with direct conductivity detection.

Determination of methylamine in the presence of sodium, ammonium, potassium, magnesium, and calcium using cation chromatography with direct conductivity detection.

Determination of lithium, sodium, ammonium, zinc, potassium, magnesium, and calcium impurities in syringe filters using cation chromatography with direct conductivity detection.