응용 분야 및 기법

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.

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.

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.

Stamps are cultural heritage objects that provide an invaluable amount of historical information. There is an increase of counterfeit historical inks and it is imperative that fraudulent stamps can be identified and removed from the market. The portable Raman i-Raman EX® with a 1064 nm laser is used because it minimizes the fluorescence of the ink. The i-Raman EX® also has the functionality of low laser power reduction down to 1% to prevent sample burning and the Raman video microscope system analyzes the smallest of details, which is imperative for cultural heritage analysis of an 1885 historical envelope.

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.

The simultaneous ion chromatographic determination of trace-levels of lanthanides (or lanthanoides) was achieved by using either direct non-suppressed conductivity detection or UV/VIS detection after post-column reaction (PCR) with arsenazo III at 655 nm. Conductivity detection under isocratic conditions resulted in an overall analysis time of approx. 70 minutes. In contrast, the determination of the lanthanides via gradient elution and subsequent spectrophotometric detection of the arsenazo III-lanthanide(III) complexes was performed within 22 minutes. Besides the outstanding analysis time, UV/VIS detection excelled by its enhanced selectivity and sensitivity and did not suffer from interferences by ubiquitous non-lanthanide impurities such as iron(III) or other transition metals. For both conductivity and spectrophotometric detection, the inclusion of sample preconcentration steps lowered the limit of detection (LOD) to the sub-ppb range.

The combination of 850 Professional IC, 858 Professional Sample Processor, Dosino and MagIC NetTM software offers a variety of sophisticated ion chromatographic sample preparation techniques. One of these is the automated inline dilution of samples.After the first sample injection, MagIC NetTM verifies if the area of the sample peak lies within the calibration range. If the measured peak area is outside these limits, the software calculates the appropriate dilution factor, dilutes and automatically re-injects the sample. For all investigated ions (Li+, Na+, K+, Ca2+, Mg2+, F-, Cl- , NO2-, Br-, NO3-, SO42- ), automated logical dilution yielded coefficients of determination (R2) better than 0.9999. Direct-injection recoveries for cations and anions were within 98.6…99.5% and 93.4…100.4% respectively. In contrast, after logical dilution, recoveries for cations and anions were within 100.1…102.9% and 98.2…102.6% respectively. The relative standard deviations for all determinations involving diluted sample solutions were smaller than 0.91%.

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.

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.

Ag electrodes are used for the indication of the potentiometric endpoints in precipitation titrations between silver and halide or sulfide ions. A coating on the silver ring may increase the sensitivity of the electrode and can thus reduce the limit of detection. This is why a variety of coated Ag electrodes are commercially available. This bulletin describes how the silver ring of Ag electrodes can be coated with AgCl, AgBr, AgI or Ag2S by electrolysis.

It is essential to know before starting the sample analysis if the electrode is in a good state or not. A well workingelectrode will increase the quality of your results, as the accuracy and precision will be increased. Furthermore, tedious error tracking can be omitted and no sample is wasted due to a defect or old electrode. There exist several ways how to check metal electrodes, e.g., measurement of redox potentials, potentiometric titration or bivoltammetric titration. This bulletin describes the best methods for the various by Metrohm available metal electrodes.

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;

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.

This Application Note outlines GITT, a key technique for studying Li-ion battery kinetics, OCV, and diffusion, using INTELLO for streamlined control and analysis.

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.

This application shows how EIS, combined with INTELLO and NOVA, tracks changes in internal battery resistance across SOC levels to study performance and aging mechanisms.

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.

Long-term determination of standard cations with automatic inline eluent preparation using Dosino and Level Control instruments and cation chromatography with direct conductivity detection.

Calibration of lithium, sodium, ammonium, zinc, potassium, magnesium, and calcium using the partial loop technique and cation chromatography with direct conductivity detection. This technique allows a calibration range of 1:100 (e.g. 1 μg/L to 100 μg/L corresponding to 2 μL to 200 μL injected volume) out of 1 calibration solution. Applying the full range of partial loop injection to the samples one calibration covers a sample concentration range of 1 to 10'000 e.g. 2 μL of a 10 mg/L solution corresponds to the highest calibration level (100 μg/L) while 200 μL of a 1 μg/L solution corresponds to the lowest calibration level.

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

Determination of monoethanolamine (MEA), diethanolamine (DEA), and triethanolamine (TEA) in the presence of lithium, sodium, ammonium, potassium, calcium, and magnesium using cation chromatography with direct conductivity detection.

Determination of monomethylamine (MMA), dimethyl-amine (DMA), and trimethylamine (TMA) in the presence of lithium, sodium, ammonium, potassium, cesium, calcium, and magnesium using cation chromatography with direct conductivity detection.

Determination of lithium, sodium, ammonium, potassium, manganese, calcium, magnesium, strontium, and barium using cation chromatography with direct conductivity detection.

Eluent preparation on demand (EPOD) is the convenient and flexible way of automatic eluent preparation. The 849 Level Control together with an 800 Dosino equipped with a 50 mL dosing unit are used to dilute an eluent concentrate to the required eluent concentration. The use of eluent concentrates is suitable for any eluent. This facilitates unattended operation of the system over several weeks (see AN S-296 for anion eluent preparation).

Metrohm intelligent Partial Loop Technique (MiPT) is a versatile injection mode in IC. In this application, injection volumes range from 4 to 200 µL (corresponding to 0.5 - 10 mg/L) using the 250 µL loop. Here, the use of 2 and 5 mL Dosing Units are compared.

The Metrosep C 6 columns have a higher capacity than those of the Metrosep C 4. The present Application Note describes the exceptional separating efficiency for standard cations with the three Metrosep C 6 column lengths available. The outstanding sodium-ammonia separation is particularly noteworthy.

Sample dilution is a work-intensive routine task in the analysis laboratory. An automatic two-step dilution exponentiates the dilution factor – 1:100 – thus incorporating a dilution factor of 10,000. The intelligent dilution is made possible by MagIC Net, which calculates the essential dilution steps, and by the dosing properties of the 800 Dosino and the Liquid Handling Station. The Application Note shows statistical results of a 1:10,000 dilution.

Fast IC means short run times on separation columns with a relatively high flow rate and the standard eluent. Here the standard cations are separated within eleven minutes on the Metrosep C 4 - 250/2.0. The sodium and ammonium peaks are separated from one another under these conditions.

Fast IC means short run times on separation columns with a relatively high flow rate. Separation with the Metrosep C 4 - 150/2.0 is even quicker than that in the AN-C-150 at 1.1 mL/min. Here, the standard cations are separated within five minutes. Under the selected conditions, sodium and ammonium are no longer completely separated.

Fast IC means short run times and a high sample throughput on columns with a relatively high flow rate and the standard eluent. Mono-, di- and tri-ethanolamine are separated with the Metrosep C 4 - 150/2.0 within 2.5 minutes.

Fast IC means short run times and a high sample throughput on columns with a relatively high flow rate and the standard eluent. Mono-, di- and trimethylamine are separated with the Metrosep C 4 - 150/2.0 within four minutes.

The high-capacity Metrosep C 6 - 150/4.0 cation column convinces with outstanding separations, narrow peaks, and a multitude of available eluents. In this Note, the selectivity for alkali, earth alkali, and certain transition metals, in addition to methyl and ethanol amines, is shown using a nitric acid eluent and direct conductivity detection.

The column temperature influences the duration of the cation separation on the high-performance Metrosep C 6 - 150/4.0 column. The retention times of lithium, sodium, ammonium, magnesium, and calcium remain practically constant with increasing column temperature, whereas those of potassium, strontium, and barium are considerably shortened. This means that the temperature can be used to reduce analysis time considerably on the Metrosep C 6 - 150/4.0.

Intelligent Inline Preconcentration with Inline Matrix Elimination (MiPCT-ME) is used for trace determination of the six standard cations in addition to zinc and diethylamine. The analysis is completed within 24 minutes on the Metrosep C 4 - 250/2.0 Microbore column. The recovery rates are in excess of 95%. The detection limits calculated with the MagIC Net software are in the lower ng/L range for a preconcentration volume of 4 mL.

Parallel anion and cation analysis is typically used when both anions and cation have to be analyzed in a sample. Here, the cation part of such an analysis is given. The sample is injected to the cation channel by the injector of the IC instrument bypassing the injector on the 889 IC Sample Center. The whole system is controlled by Empower applying the Metrohm IC Driver 2.0. For anion analysis, see AN-S-350.

Automatic dilution reduces manual work and improves the reproducibility and accuracy of the results. So far, the Inline Dilution Technique (MIDT) has been tested in a range of max. 1:100. Using a dedicated sample needle this range is enlarged significantly. This AN shows the performance of an Inline Dilution with a factor of 1:2000 as well as a comparison of manual and inline dilution for a dilution factor of 1:1000.

AOF (adsorbable organic fluorine) is used to screen for per- and polyfluorinated alkyl substances in aqueous matrices via pyrohydrolytic combustion and ion chromatography.

Combustion ion chromatography (CIC) measures AOX (adsorbable organically bound halogens, i.e., AOCl, AOBr, AOI) and AOF as well as CIC AOX(Cl) according to DIN 38409-59 and ISO 18127.

A corrosion inhibitor is a substance that reduces the corrosion rate of a metal. A corrosion inhibitor is usually added in a small concentration to the corrosive environment. This application note shows how Metrohm Autolab instruments can be used to check the quality of inhibitors.

Corrosion of metals is a problem seriously affecting not only many industrial sectors, but also private life, resulting in enormous costs. In this application note, the results gained during electrochemical corrosion studies on different metals are compared to literature data.

The ASTM standard G100 is an electrochemical method to test localized corrosion of aluminum 3003-H14 and other alloys. A cyclic galvanostatic staircase polarization (galvanostaircase) is composed of an upward and a downward scan. The potential values at the end of each step are collected and linearly fitted, and the potential values at zero current are found.

This Application Note evaluates corrosion in Type 430 stainless steel according to ASTM G5 with VIONIC powered by INTELLO and an ASTM-compliant corrosion cell setup.

The rotating cylinder electrode (RCE) is successfully used in a laboratory environment to generate a turbulent flow at the surface of a sample, simulating realistic pipe flow conditions. In this application note, the corrosion rate is measured and compared between quiescent and turbulent flow conditions, while keeping all the other experimental conditions unchanged. The linear polarization (LP) technique was used together with the RCE (with and without rotation).

This Application Note details ASTM G61-compliant corrosion measurements performed with VIONIC powered by INTELLO using Metrohm’s ASTM-compliant corrosion cells.

The ASTM B825 is used to determine the corrosion and tarnish film on metal surfaces. This is achieved by using the so-called cathodic reduction method. With the help of a Metrohm Autolab PGSTAT302N and a Metrohm Autolab 1 L corrosion cell, a procedure to replicate the ASTM B825 is shown.

Tafel analysis is an important electrochemical technique used to understand reaction kinetics. By studying the Tafel slope, it reveals the rate-determining steps in electrode reactions, aiding fields like corrosion and fuel cell research. This method helps industries optimize processes and improve device performance by tailoring materials and conditions for greater efficiency.

Cation chromatography with sequential suppression enables the determination of cations in their hydrogen carbonate form. The eluent – usually nitric acid – is converted into carbonic acid. Following its decomposition into carbon dioxide and water, the former is continuously removed by the CO2 suppressor. The reduction of baseline noise thus achieved permits the lowering of the detection limits and improves reproducibility, even at very low cation concentrations. This Note shows the reproducibilities determined for cation concentrations of 10 µg/L.

Ammonium determination after sequential suppression frequently exhibits non-linear calibration curves. The reason for this is the ammonium hydroxide that arises and that is present in a form characterized by low dissociation. The sequential cation suppression forms the more highly dissociated ammonium hydrogen carbonate. Ammonium and the other standard cations exhibit linear calibration curves (R > 0.9997).

This Application Note shows the selectivity of the Metrosep C Supp 1 - 250/4.0 column for alkyl and ethanol amines in addition to standard cations under isocratic conditions. Quantification takes place using conductivity detection following sequential suppression.

Electrochemistry, spectroscopy, and spectroelectrochemistry (SEC) are widely used techniques in many fields. However, the data curves obtained from these analyses are quite varied, and not all electrochemical peaks and spectroscopic bands can be measured with the same procedures. This Application Note examines four tools included in the DropView 8400 and DropView SPELEC softwares to facilitate the measurement and analysis of the collected curves and data. The following measurement options are explained in detail: automeasurement, set on curve measurement, set free measurement, and set step measurement.

The mass transport characteristics of the diffusion controlled oxidation and reduction of the ferri/ferro cyanide couple was studied using the Autolab RDE with a low noise liquid Hg contact.

A reference electrode has a stable and well-defined electrochemical potential (at constant temperature), against which the applied or measured potentials in an electrochemical cell are referred. A good reference electrode is therefore stable and non-polarizable. In other words, the potential of such an electrode will remain stable in the used environment and also upon the passage of a small current. This application note lists the most used reference electrodes, together with their range of use.

This application explains ohmic iR drop in electrochemical cells, its causes, and strategies to minimize its impact for accurate and reliable potential measurements.

This application introduces two tools (current interrupt and positive feedback) that measure and compensate for up to 90% of the ohmic iR drop, a common error in electrochemistry.

The Autolab Electrochemical Quartz Crystal Microbalance (EQCM) is an optional module for the Autolab PGSTAT which can be used to control a 6 MHz crystal oscillator. This technique can be used to perform electrogravimetric measurements with detection limits in the sub μg range.

This document describes a very simple procedure that can be used to produce small deposits of platinum on a goldsubstrate. This simple procedure is based on an electrochemical process known as displacement deposition, during which the deposition of a noble metal occurs by the oxidation of a precursor metal adlayer deposited on the substrate, at open circuit potential (OCP).

In this Application Note, analog and digital staircase potential signals are applied to a platinum working electrode in an acidic solution. The differences in measured currents are highlighted and compared with a similar experiment where the current is being calculated from the measured charge.

A basic overview of the working principle of a potentiostat/galvanostat is presented. Depending on the application, the connections of the instrument to the electrochemical cell can be (or must be) set up in different ways. Below, the three commonly used electrochemical cell setups are discussed together with the role of the electrodes used in electrochemical measurements.

In this application note, the combination between electrochemistry and spectroscopy is shown, with the oxidation of ferrocyanide to ferricyanide monitored with IR spectra taken at defined potential steps. The increase in absorbance at 425 nm corresponding to the formation ferricyanide.

To improve the performance of electrochemical energy storage devices like batteries and supercapacitors, one can focus on enhancing the ion conductivity (ƠDC) of the electrolyte. It is a common method for obtaining ƠDC values of different electrolyte systems, to carry out electrochemical impedance spectroscopy (EIS) experiments, at different temperatures, in a 2-electrode setup.

Copper is arguably one of the most technologically relevant metals, especially for the semiconductor industry. The deposition process used in this industry is known as the dual-damascene process and it involves the electrodeposition of copper from an acidic cupric compound, in the presence of additives.This Application Note illustrates the use of the Autolab rotating ring disc electrode (RRDE) for the study of electrodeposition of copper and the detection of the Cu+ intermediate.

The relative permittivity εr, also known as dielectric constant, is of great importance in materials characterization. It can be defined as the ratio between the amount of electrical energy stored in a material and the amount of electrical energy stored in a vacuum. One of the easiest way to obtain the relative permittivity is to calculate it from capacitance values. In this Application Note, five techniques to retrieve capacity values have been compared.

In this application note, electrochemical impedance spectroscopy (EIS) is used to test a commercial battery connected in two different ways. In the first EIS measurement, the battery is connected in a two-terminal sensing configuration. In the second EIS measurement, the battery is connected in a four-terminal sensing (Kelvin sensing) configuration. The difference in how the leads are connected results in different measured impedance values for the battery.

The oxygen reduction reaction (ORR) is important to the functional readiness of a fuel cell. Rotating ring disk electrode (RRDE) experiments allow the reaction to be studied in hydrodynamic conditions to determine kinetic properties via the Levich and Koutecký-Levich equations. Mechanistic information is simultaneously obtained from the reaction of intermediates at the secondary (ring) electrode. This application note describes how the RRDE from Metrohm Autolab can be used to study the ORR.

The TSC SW Closed and TSC Battery cells are compact systems designed for measurements on air or moisture-sensitive materials, such as those used in batteries. In this document, two testing procedures are explained. The first procedure is withpotentiostatic cyclic voltammetry (CV), while the second is via electrochemical impedance spectroscopy (EIS).

Convolution voltammetry consists essentially of a voltammetric, chronoamperometric, or chronocoulometric experiment followed by a mathematical transformation - convolution. Using a convolution method, the effect of the decrease of the concentration gradient can be eliminated from the total response of the electrode. This application note explains how the convolution in NOVA works.

In order to calculate the conductivity of an electrolyte, the cell constant of the cell must be known. The combination of the Metrohm Autolab PGSTAT204 equipped with the FRA32M module in combination with the Autolab Microcell HC setup was used for the determination of the conductivity cell constants of TSC1600 temperature controlled electrochemical cell.

The proton conductivity of membranes made of a proton conductive material is an essential quantity to be determined. In this application note, we present the results of an exemplary study of σDC(T) determined by impedance spectroscopy for a novel solid proton conductor in its dry state.

The kinetic and mass transfer parameters of the electro-oxidation reaction of TEMPO were measured using the TSC Surface measuring cell for the Autolab Microcell HC system. The cell allows the study of electrochemical processes in liquid electrolytes in a three electrode configuration under temperature control.

The study of the electrochemical behavior of platinum in acidic media is of crucial importance in fundamental electrochemistry and electrocatalysis. Most electrocatalytic processes occurring at Pt electrodes are highly sensitive to the structure of the platinum surface. Cyclic voltammetry (CV) is a widely used rapid measurement technique that provides both a qualitative and quantitative fingerprint of platinum surfaces. A comparison of results given by linear and staircase CVs is presented in this Application Note.

Many different configurations are made possible when using two-, three-, or four-electrode cell setups in research. Depending on the experimental requirements, one setup may be preferred over another. Therefore, the proper electrode arrangements for these three situations are defined in this Application Note. As an example, the potential at the counter electrode is measured during the platinum oxidation in acidic media, with the second sense (S2) of VIONIC powered by INTELLO. Since dissolved Pt in solution could bias the results, it is important to be able to monitor the potential of the counter electrode.

In this Application Note, the electrochemical properties of electrodes with a micrometer-size surface area are compared with the electrochemical properties of electrodes with millimeter-size surface area. The comparison is made through cyclic voltammetry in a Fe3+/Fe2+ (ferro/ferri) solution, and the differences in the voltammograms are explained with the different diffusion profiles at the electrode-electrolyte interface.

This Application Note highlights the use of Metrohm Hyphenated EC-Raman Solutions to monitor the reversible oxidation of ferrocyanide at a gold electrode.

This Application Note presents a walkthrough of an experiment on 4-nitrothiophenol using hyphenated EC-Raman, a combination of Raman spectroscopy and electrochemistry.

Advances in polymeric membranes and screen-printed technologies have enabled miniaturized, portable potentiometric sensors ideal for point-of-care analysis.

By using an enzymatic sensor with a screen-printed electrode, producers can measure lactic acid production, thereby monitoring fermentation processes.

This Application Note explains manual and automated iR drop correction with electrochemical impedance spectroscopy and cautions against using less accurate methods.

Spectro electrochemiluminescence experiments comparing photodiode and microspectrometer detectors, showing how each sensor captures ECL signals for the analysis of single and dual luminophore systems.

This Application Note presents an electrochemiluminescence (ECL) method for a fast, accessible, and cost-effective alternative method to detect fentanyl.

This application note demonstrates EQCM D for simultaneous mass and dissipation analysis of Ni(OH)₂ electrodeposition.

Electrochemical impedance spectroscopy (EIS) is a widely used multidisciplinary technique for characterizing the behavior of complex electrochemical systems. EIS is employed in the study of a range of complex systems including batteries, catalysis, and corrosion processes. This Application Note focuses on the basic principles of EIS measurements.

A typical electrochemical impedance spectroscopy (EIS) experimental setup consists of an electrochemical cell, a potentiostat/galvanostat, and a frequency response analyzer (FRA). This Application Note introduces common EIS experimental setups as well as details of the main experimental parameters.

Here, the most common circuit elements for EIS are introduced which may be assembled in different configurations to obtain equivalent circuits used for data analysis.

Explore how to construct simple and complex equivalent circuit models for fitting EIS data in this Application Note. Nyquist plots are shown for each example.

In the application note AN-EIS-004 on equivalent circuit models, an overview of the different circuit elements that are used to build an equivalent circuit model was given. After identifying a suitable model for the system under investigation, the next step in the data analysis is estimation of the model parameters. This is done by the non-linear regression of the model to the data. Most impedance systems come with a data-fitting program. In this application note, the way NOVA is uses to fit the data is shown.

In this application note, the advantage of recording the raw time domain data for each individual frequency during an electrochemical impedance measurement is described.

This Application Note presents the Mott-Schottky measurement, an extension of electrochemical impedance spectroscopy (EIS), on a popular semiconducting material.

A fuel cell is an electrochemical energy conversion device that produces electricity and heat by electrochemically combining a fuel (typically hydrogen) and an oxidant (typically oxygen). The higher efficiency also results in much lower carbon dioxide emissions and negligible amounts of SOx and NOx (when reformed fuel is used) compared with fossil fuel-based technologies for the same power output.

To overcome the various technical problems, many different fuel cell types have been developed. In this Application Note, proton exchange membrane, direct methanol and solid oxide fuel cells are discussed in more detail.

In this Application Note the use of Electrochemical Impedance Spectroscopy (EIS) for the characterisation of PEM fuel will be demonstrated. It will be shown that EIS is a powerful diagnostic tool for the determination of the following factors that can influence the performance of a PEM fuel cell.

In this application note, a combination of PGSTAT and electronic load is use to perform electrochemical impedance spectroscopy in a fuel cell operating at high currents.

The use of impedance measurements on fuel cells under load makes it possible to study the influence of the different fuel cell elements on the behavior and (if detectable) on the ageing of the fuel cell. To perform high current density measurements, the Autolab systems can be connected to a third party electronic load. This extends the measurable range of the instrument by several current decades.

The operational behavior of a fuel cell stack is usually evaluated by determining the polarization and power density curves of the cell. These curves provide a quick characterization of the stack performance and an assessment of its optimal operating conditions (temperature, humidity, electrocatalyst, ion-exchange membrane).

In recent years, field-effect transistors (FETs) have become more commonly used as a sensing platform for a multitude of electrochemical and biological applications. These devices are promising bioelectronic transducers that allow both low-potential operation and stable potentiometric measurements. FETs are now seen as an attractive alternative to using conventional electrochemical detection systems in the scientific community. This Application Note gives in-depth guidance about how to operate Metrohm DropSens bipotentiostat devices for the characterization of FETs and their use as transducers. A single μStat-i 400 device, a small and portable bipotentiostat and galvanostat, is used to demonstrate the experiments.

In this Application Note, the Metrohm DropSens SPELEC instrument is used with the FLUORESCENCE KIT for time-resolved monitoring of electrochemical reactions in a semi-infinite diffusion regime by performing fluorescence spectroelectrochemistry of the [Ru(bpy)3]2+/3+ redox couple.

Alamar Blue is monitored with fluorescence spectroelectrochemistry during its irreversible reduction to resorufin and further reversible reduction to dihydroresorufin.

Standardisation of sodium tetraphenylborate (NaTPB) solution for the determination of potassium and for nonionicsurfactants.

Standardization of 0.1 mol/L in propan-2-ol for use in applications for the determination of weakly acidic species in non-aqueous media.

Standardization of 0.1 mol/L ammonium ferrous sulfate solution for use in thermometric titration of Cr(VI) solutions.

Standardization of cetyl pyridinium chloride solutions for use as a cationic surfactant titrant in the determination ofanionic surfactants such as sodium lauryl ether sulfate.

This Application Note discusses the standardization of thiosulfate titrant for use in the determination of copper with thermometric titration.

Thermometric complexometric titration of metals is often performed with tetrasodium EDTA. This Application Note explains the standardization of tetrasodium EDTA titrant with copper.

This Application Note explains how to use magnesium to standardize tetrasodium EDTA titrant.

Standardization of copper back-titrant using standard tetrasodium EDTA titrant in the determination of metals.

Standardization of disodium dimethylglyoximate by thermometric titration with standard Ni(II) solution.

Standardization of barium acetate titrant used in the determination of sulfate in phosphoric acid. The same procedure is applied if barium chloride is chosen as the titrant.

Standardization of sodium fluoride titrant for determination of aluminum.

Standardization of 0.1mol/L perchloric acid in glacial acetic acid by catalyzed endpoint thermometric titration.

Standardization of titrant for direct determination of sodium.

Determination of bicarbonate and carbonate in a mixture by sequential thermometric titrations.

Standardization of ~1mol/L tetrasodium EDTA solutions for thermometric complexometric analysis.

This Application Note outlines the determination of total acidic active surface sites in zeolites with thermometric titration.

This Application Note shows that the parameter of surface basicity of zeolites can be measured by thermometric titration.

Standardization of 1 mol/L tetrasodium EDTA (Na4EDTA) solutions by titration with standard magnesium solution.

This Application Note describes in detail how to determine the blank value and the titer for thermometric titrations using tiamo™.

Ammonia determination via NH3 ISE requires precise calibration. Details on this are provided by the present Application Note.

This Application Note covers the formation of calcium carbonate from solution.

Large sample sizes can lead to subtraction of too high blank values. This Application Note describes the calculation of a relative blank and thus helps to improve the accuracy of the method.

The new DIN draft standard 38407-53 outlines TFA analysis in water using direct injection LC-MS/MS, enabling quantification from 0.1–3.0 μg/L as shown in this Application Note.

Determination of anions in a Schoeniger absorption solution of a test mixture without decomposition of the H2O2 using anion chromatography with direct conductivity detection.

Determination of cyanide using anion chromatography with amperometric detection at the silver electrode.

Determination of chromate using anion chromatography with post-column reaction and UV/VIS detection.

Determination of borate and silicate in ultrapure water using anion chromatography with direct conductivity detection.

This Application Note describes how the accuracy of your NIR measurements can be increased with instrument calibration.

This Application Note describes how the accuracy of your NIR measurements can be increased with reference standards.

This Application Note shows the transfer of near-infrared spectroscopy analysis methods from the FOSS NIRSystems System II (5000/6500) Analyzer to the Metrohm NIRS XDS und DS2500 Analyzers. In addition, the advantages of the new NIRS XDS and DS2500 analyzers with extended spectral range and improved resolution are displayed, in particular with respect to the FOSS NIRSystems System II analyzer.

Determination of lauric acid, myristic acid, palmitic acid, and stearic acid using ion-pair chromatography with direct conductivity detection.

Determination of organic acids and phosphate using ion-exclusion chromatography with direct conductivity detection.

Determination of gluconic acid and glycolic acid using ion-exclusion chromatography with direct conductivity detection.

Determination of formate, acetate, propionate, butyrate, valerate, and capronate in an aqueous absorption solution using ion-exclusion chromatography with conductivity detection after chemical suppression.

Determination of lactate, formate, acetate, propionate, butyrate, isobutyrate, valerate,and isovalerate in a standard solution using ion-exclusion chromatography with conductivity detection after chemical suppression.

Determination of glycolic acid, formic acid, glutaric acid, acetic acid, propionic acid, and butyric acid in a standard solution using ion-exclusion chromatography with suppressed and non-suppressed conductivity detection.

Determination of carbonate in an aqueous ammonia solution using ion-exclusion chromatography with suppressed conductivity detection.

Determination of formate, acetate, propionate, isobutyrate, butyrate, isovalerate, valerate, and capronate added to tap water using anion chromatography with conductivity detection after suppression. The MCS is placed upstream of the chemical suppressor to remove interfering CO2.

Determination of sulfite, nitrite, nitrate, sulfate, imidodisulfonate, and peroxodisulfate using ion-pair chromatography with conductivity detection after suppression.

Determination of carbohydrates on the column Hamilton RCX-30 - 250/4.6 using pulsed amperometric detection.

Determination of carbohydrates on the column Hamilton RCX-30 - 150/4.6 using pulsed amperometric detection.

The determination of sugar and sugar alcohols is very important for food analysis. The Dose-in Gradient system extends the gradient capability of the standard IC system. The isocratic system is expanded to form a binary gradient system with just one 800 Dosino and one T-piece.

This Application Note shows the determination of glucose and galactose in a 2% solution of lactose. The separation is achieved on a Hamilton RCX-30 - 250/4.6 applying pulsed amperometric detection (PAD) at a gold electrode. Instrument control, data acquisition, and data handling is done by Empower 3.0 using the Metrohm IC Driver 2.0 for Empower.

Worldwide, milk and dairy products are vital sources for human nutrition. A major component and energy source in dairy products is lactose. To efficiently metabolize lactose, the enzyme lactase is indispensable. However, globally nearly 70% of the population is lactose intolerant and they have difficulties to digest lactose. Lactose malabsorption leads to numerous gastrointestinal and extra-intestinal symptoms and other complaints with varying extents. Therefore, consumers rely on accurate food labels and for manufacturers appropriate sensitive analytical techniques are a must to comply with these demands. Ion chromatography with pulsed amperometric detection (IC-PAD) enables the determination of very low lactose contents. Validation according to AOAC requirements shows the high sensitivity and reliability of this method as a routine analysis.

Dye-sensitized solar cells (DSC) are currently subject of intense research in the framework of renewable energies as a low-cost photovoltaic (PV) device. To characterize photovoltaic devices, two additional frequency domain methods can be used, based on the modulation of the light intensity. These two methods are Intensity modulated photovoltage spectroscopy (IMVS): measurement of the transfer function between the modulated light intensity and the generated AC voltage, and Intensity modulated photocurrent spectroscopy (IMPS): measurement of the transfer function between the modulated light intensity and the generated AC current.This Application Note illustrates the use of the Metrohm Autolab PGSTAT302N equipped with a FRA32M module, in combination with the Autolab Optical Bench kit to perform IMVS and IMPS characterization of photovoltaic devices.

This application note shows how it is possible with Metrohm Autolab PGSTATs and the Metrohm Autolab Optical Bench, to retrieve information about the mechanism and the kinetics of the back reaction, a side reaction which limits the performances of dye-sensitized solar cells.

In this document, a procedure to calibrate the LED light of the Metrohm Autolab Optical Bench is presented. The procedure can be applied to the single-wavelength LED lights. Calibration is performed in order to relate the LED light intensity to the LED driver current. In this way, it is possible to correct the light intensity values when the distance between the solar cell under test and the LED light is changed. Additonally, the calibration allows the user to perform measurements on solar cells while specifying the light intensity values, instead of the LED driver current.

This Application Note presents the procedure to determine the responsitivity value for calibrating the white lights of the Metrohm Autolab Optical Bench.

Carbon materials are a remarkable choice as electrode surfaces. They are not only cost-effective and chemically inert, but also have a low background current and a wide potential window. Physical and chemical properties of new carbon nanomaterials depend mainly on their structure, so their characterization is essential to choose the right material for different applications.Raman spectroscopy is a very attractive technique for this purpose, effortlessly distinguishing information about the bond structure of carbon materials, and, therefore, about their possible properties. DropSens screen-printed electrodes (SPEs) are low-cost, disposable devices, available with working electrodes fabricated in several carbon materials. This Application Note describes how their properties can be studied by Raman spectroscopy.

Substrates for surface-enhanced Raman spectroscopy (SERS) are typically fabricated with complex (micro/nano)structures of noble metals, enabling trace level detection of analytes. Due to the high costs and reactivity of these SERS substrates, they often have a limited shelf life. Development of new substrate materials which minimize these issues yet maintain the same performance standards is a constant concern.Screen-printed electrodes can be easily fabricated using different metallic materials with the well-established screen-printing method, leading to mass production of versatile, cost-effective, and disposable devices. In this Application Note, the feasibility of using readily-available screen-printed metal electrodes as suitable substrates for the fast and sensitive detection of different chemical species by in situ electrochemical SERS (EC-SERS) is shown.

Spectroelectrochemistry is a multi-response technique that provides both electrochemical and spectroscopic information about a chemical system in a single experiment, i.e., it offers information from two different points of view. Spectroelectrochemistry focused on the UV/VIS region is one of the most important combinations because this allows us to obtain not only valuable qualitative information, but also outstanding quantitative results. In this application note, the degradation kinetics for 4-nitrophenol, a known pollutant, were determined using SPELEC.

Spectroelectrochemistry is a multi-response technique that provides electrochemical and spectroscopic information about a chemical system in a single experiment, i.e., it offers information from two different points of view. Raman spectroelectrochemistry could be considered as one of the best techniques for both the characterization and behavioral understanding of carbon nanotube films, as it has traditionally been used to obtain information about their oxidation-reduction processes as well as the vibrational structure. This application note describes how the SPELEC RAMAN is used to characterize single-walled carbon nanotubes by studying their electrochemical doping in aqueous solution as well as to evaluate their defect density.

Many electrochemical methods have been developed but are traditionally limited to aqueous media. Raman spectroelectrochemistry in organic solutions is an interesting alternative, but developing new EC-SERS procedures is still required. This Application Note demonstrates that the electrochemical activation of gold and silver electrodes enables the detection of dyes and pesticides in organic media.

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.

Low sensitivity has limited the use of Raman spectroscopy as a detection method. However, the surface-enhanced Raman scattering (SERS) effect has improved its effectivity for analytical use. Aldehyde dehydrogenase (ALDH) and cytochrome c are analyzed by Raman spectroelectrochemistry as a proof of concept in this Application Note.

This Application Note compares SPELEC RAMAN and a standard Raman instrument by analyzing their performance in measuring single-walled carbon nanotubes (SWCNT).

EC-SERS enhances Raman sensitivity using electrochemically activated gold SPEs, enabling rapid, simplified pesticide detection without complex prep or instrumentation.

Metrohm’s MIRA XTR handheld Raman spectrometer enables fast, reagent-free identification of phosphate species, enabling continuous monitoring of dynamic systems.

Raman spectroscopy with PLS modeling enables rapid, accurate, nondestructive quantification of the total phosphate content in solution with minimal sample preparation.

Low frequency Raman spectroscopy extends conventional Raman analysis by capturing vibrational modes down to 65 cm-1, enabling deeper insights into molecular structure, protein characterization, polymorph identification, and phase changes.

Determination of chloride, sulfate, oxalate, and fumarate using anion chromatography with conductivity detection after chemical suppression.

Separation of fluoride, chloride, nitrite, bromide, nitrate, phosphate, phosphite, sulfate, and tetrafluoroborate using anion chromatography with conductivity detection after chemical suppression.

Determination of 1 (3) µg/L of chloride, nitrite, bromide, nitrate, phosphate, and sulfate after direct injection using anion chromatography with conductivity detection after chemical suppression.

Reproducibility of fluoride, chloride, nitrite, bromide, nitrate, and sulfate in the ppb range using anion chromatography with conductivity detection after chemical suppression.

Determination of acetate, chloride, nitrite, nitrate, benzoate, phosphate, and sulfate using anion chromatography with conductivity detection after chemical suppression.

Determination of traces of fluoride, chloride, nitrate, phosphate, and sulfate in 15% NaOH using anion chromatography with conductivity detection after chemical suppression and inline sample neutralization.

Determination of acetate, monochloroacetate, and dichloroacetate using anion chromatography with conductivity detection after chemical suppression.