Aplikace

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.

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

UV/VIS detection is one of the most sensitive detection techniques in trace-level chromatography. Sometimes, however, spectrophotometric detection lacks sensitivity, selectivity or reproducibility and chemical derivatizations are required. By using Metrohm`s rugged and versatile flow-through reactor, single- or multi-step derivatizations can be done fully automatically, in either pre- or post-column mode at any temperature between 25…120 °C. The variable reactor geometry allows to adjust the reactor residence time of the reactants according to derivatization kinetics. The flexibility of the reactor is demonstrated by optimizing four widespread post-column techniques: the relatively slow ninhydrin reaction with amino acids and the fast derivatizations of silicate, bromate and chromate(VI).

The presented IC system with inline sample preparation allows the determination of traces of lithium and sodium (ppt) in the presence of ppm quantities of ammonium and ethanolamine.

The Combustion IC system presented allows the automated determination of organic halogen and sulfur compounds in all flammable samples. Both combustion digestion, which is automatically controlled with a flame sensor, and the professional Liquid Handling guarantee highest precision and trueness. This poster describes the determination of the halogen and sulfur content in a certified polymer standard, a coal reference material as well as in latex and vinyl gloves.

Boric acid is used in many primary circuits of nuclear power plants, in nickel plating baths, and in the production of optical glasses. Furthermore, boron compounds are found in washing powders and fertilizers. This bulletin describes the potentiometric and thermometric determination of boric acid. The determination also covers further boron compounds, when acidic digestion is applied.

The photometric determination of nitrate is limited by the fact that the respective methods (salicylic acid, brucine, 2,6-dimethyl phenol, Nesslers reagent after reduction of nitrate to ammonium) are subject to interferences. The direct potentiometric determination using an ion-selective nitrate electrode causes problems in the presence of fairly large amounts of chloride or organic compounds with carboxyl groups. The polarographic method, on the other hand, is not only more rapid, but also practically insensitive to chemical interference, thus ensuring more accurate results. The limit of quantification depends on the matrix of the sample and is approximately 1 mg/L.

Sulfide and sulfite can be determined polarographically without any problems. For sulfide, polarography is performed in an alkaline solution, for sulfite in a slightly acidic primary solution. The method is suitable for the analysis of pharmaceuticals (infusion solutions), wastewater/flue gas water, photographic solutions, etc.

Only coulometric Karl Fischer titration can determine low water contents with sufficient accuracy.This Application Bulletin describes the direct determination according to ASTM D6304, ASTM E1064, ASTM D1533, ASTM D3401, ASTM D4928, EN IEC 60814, EN ISO 12937, ISO 10337, DIN 51777, and GB/T 11146. The oven technique is described according to ASTM D6304, EN IEC 60814, and DIN 51777.

This Bulletin describes the fully automated determination of uranium according to the method of Davies and Gray: Uranium(VI) is reduced in concentrated phosphoric acid solution with iron(II) to form Uranium(IV). With molybdenum as a catalyst, the excess iron(II) is oxidized with nitric acid. The nitrous acid that is formed is destroyed with sulfamic acid before uranium(IV) is titrated with a potassium dichromate solution in the presence of a vanadium catalyst.

Chlorine is frequently added to drinking water for disinfection. Depending on the reactivity and the concentration of chlorine, toxic disinfection by-products (DBPs) can thereby be released. Therefore, it is necessary to strictly control the chlorine concentration in the drinking water. This Application Bulletin shows how to determine the chlorine concentration according to three standard methods: DIN EN ISO 7939-1, APHA 4500-Cl Method B, and APHA 4500-Cl Method I.

This bulletin deals with the automated determination of mixtures of HNO3, HF and H2SiF6 in the range of approximately 200-600 g/L HNO3, 50-160 g/L HF, and 0-185 g/L H2SiF6 using thermometric titration.Etch acid mixtures containing HNO3, HF and H2SiF6 from the etching of silicon substrates can be analyzed in a sequence of two determinations using the 859 Titrotherm. The first determination involves a direct titration with standard c(NaOH) = 2 mol/L, followed by a back titration with c(HCl) = 2 mol/L. This determination yields the H2SiF6 content plus a value for the combined (HNO3+HF) contents. The second determination consists of a titration with c(Al3+) = 0.5 mol/L to determine the HF content. For freshly made up mixtures of HNO3 and HF containing no H2SiF6, a linked two-titration sequence is employed. Results from the two determinations are used by tiamoTM to yield individual results for HNO3, HF and H2SiF6.

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.

A nickel metal hydride battery, abbreviated NiMH, is a type of rechargeable battery similar to a nickel-cadmium (NiCd) battery but, for the anode, instead of cadmium, it has a hydrogen absorbing alloy. Like in NiCd batteries, nickel is the cathode. The voltage output of such packs is directly proportional to the number of single cells in the pack. In some cases, the total voltage can exceed the maximum of 10 V that is measurable by the Autolab potentiostat/galvanostat. To apply and measure voltages greater than 10 V, we have developed a voltage multiplier that increases the voltage range of the Autolab.

Lithium-ion (Li-ion) batteries are one of the most important energy storage devices in the market. A typical Li-ion battery is usually composed of one or more cells. Characterization of Li-ion cells and batteries usually involves the galvanostatic charge and discharge during various cycles.

This Application Note shows how AUTOLAB and NOVA is used to perform GITT tests on a Li-ion battery. Here,galvanostatic charge pulses are applied, each followed by relaxation time, until the upper potential limit is reached. Then, discharge pulses are applied, followed by equilibration time, until the lower potential limit is reached. From the potential vs. time plot, important information for calculating the diffusion coefficient and thermodynamics parameters quantities can be obtained.

During charge and discharge of a Li-ion battery, lithium ions are transported from one electrode through the electrolyte to the other electrode. Knowing the chemical diffusion coefficient of electrode materials is crucial. The potentiostatic intermittent titration technique (PITT) is one of the most used techniques to retrieve insights on the diffusion coefficient of the electrode active materials.

The main components of a battery are the positive and negative electrodes, together with the electrolyte, which provides only the ionic conductivity. The most common electrolytes are in the liquid state. Therefore, a separator is needed to provide a physical separation between the electrodes. The separator is soaked with electrolyte. The MacMullin number is a parameter used to determine the quality of a separator, in terms of ionic conductivity, when soaked with an electrolyte. The MacMullin number can be calculated, using the results of data fitting of two EIS experiments and the geometric factors of the measurement cells. In this application note, a commercial electrolyte is employed, together with a porous filter, used as a separator.

The TSC SW closed and TSC battery cells are compact systems designed for measurement of air or moisture sensitive materials, such as those materials used in rechargeable batteries. These cells offer well-controlled environment for the in-temperature measurement of solid and gel like materials in contact with metal electrodes in planar geometry. For example, battery active materials, ionically conductive solid-state electrolytes and battery separators can be tested using these cells. In this experiment, standard resistors of 100 Ω are used in both cells to understand the cell effects, if any, on the measurements.

The DuoCoin Cell Holder is introduced. EIS measurements on a commercial coin cell battery are performed. Differences in impedance between the four-terminal configuration and two-terminal configuration is highlighted, putting in evidence the importance of having a direct four-terminal configuration, when low-impedance DUTs are investigated.

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.

Determination of zinc, lithium, cobalt, sodium, ammonium, potassium, manganese, magnesium, and calcium in power plant feed water stabilized with 7 ppm monoethanolamine using cation chromatography with direct conductivity detection.

Determination of magnesium, strontium, and barium in produced water using cation chromatography with direct conductivity detection.

Determination of trace levels of lithium, sodium, ammonium, potassium, magnesium, and calcium in boiler feed water using cation chromatography with direct conductivity detection.

Determination of traces of zinc and iron(II) in the presence of lithium, sodium, ammonium, potassium, calcium, and magnesium in boiler water using cation chromatography with direct conductivity detection.

Methylamine (MMA), dimethylamine (DMA), and trimethylamine (TMA) in methylpyrrolidone using Metrohm Inline Matrix Elimination.

Determination of monomethylamine (MMA), dimethylamine (DMA), trimethylamine (TMA), monoethanolamine (MEA), diethanolamine (DEA), and triethanolamine (TEA) using cation chromatography with direct conductivity detection.

Determination of lithium, sodium, ammonium, and monoethanolamine (MEA) using cation chromatography with direct conductivity detection and Metrohm Inline Preconcentration and Inline Calibration.

In pressurized water reactors (PWRs), light water is used as primary coolant. Boron (as boric acid) readily absorbs neutrons and is added to the coolant to control reactivity. Lithium hydroxide assures a pH value greater than 7 to prevent corrosion. This application allows to measure sub-ppb levels of zinc, nickel, calcium, and magnesium besides high boric acid and lithium hydroxide concentrations.

Water in steel-based cooling systems requires a pH value slightly above 7 to prevent corrosion. Often ammonium or organic amines are applied for pH adjustement. This application shows the separation of typical amines besides inorganic cations. Sample preconcentration applies combined Inline Preconcentration and Matrix Elimination (MiPCT-ME).

In pressurized water reactors (PWRs), light water is used as coolant in the primary side. Boron (as boric acid) is added to the coolant to absorb neutrons, thus controlling reactivity. Lithium hydroxide assures the alkaline pH value to prevent corrosion. This application allows to measure lithium content besides high boric acid concentrations. AN-C-138 shows the respective trace metal determination on the same system setup.

Metrohm Inline Preconcentration Technique with matrix elimination (MiPCT-ME) is a powerful method that combines preconcentration, matrix elimination, and multilevel calibration. In this Application Note, the methodology is applied to the determination of traces of sodium in addition to 2 mg/L ammonia. The Metrosep C 6 - 250/4.0 column is used for selectivity reasons.

N-methyldiethanolamine and piperazine are used in scrubber solutions, e.g., in the natural gas process. Testing this type of samples by ion chromatography requires a good resolution and the separation of amines from standard cations. The separation is achieved on a Metrosep C 4 - 150/4.0 column applying direct conductivity detection.

Before the liquefaction process of the natural gas, carbonate and hydrogen sulfide need to be removed through a scrubber solution containing piperazine and N-methyl diethanolamine (MDEA). The concentration ratio of the two components is determined by ion chromatography on a Metrosep C 4 - 150/4.0 column applying direct conductivity detection.

The exploration and processing of lithium ores is gaining importance with the growing demand for lithium hydroxide. Lithium hydroxide is a key component in the manufacturing of rechargeable batteries for use in various applications including electric vehicles, home storage systems, power tools and consumer electronics. To ensure the efficiency for advanced processing of high purity lithium hydroxide, a fast and reliable quantitative detection technique is required. This application has been developed to monitor the lithium, sodium, and calcium content in the lithium processing samples and mineral concentrates.

The manufacture of ultrapure water for the pharmaceuticals industry or the semiconductor industry requires high-quality ion exchangers. Metrohm Combustion Ion Chromatography is an indispensable tool in this connection for testing the purity of anion exchange material. The output sample was wet and had to be dried at 105 °C in a special oven with waste air evacuation.Keyword: pyrohydrolysis

The burning of coal contaminates the atmosphere with halogens. Fluorine and chlorine are natural components of coal, whereas the bromide that is found therein is often adulterated as calcium bromide in order to reduce mercury emissions. This Application Note shows the results of combustion digestion with Combustion IC for three coal samples, each with a different bromide content.Keyword: pyrohydrolysis

Coal contains a certain amount of fluorine, chlorine, and sulfur compounds. During combustion of the coal, these components release corrosive acids (e.g., fluorine compounds form hydrofluoric acid). Thermal power plants therefore request low-fluorine coal to avoid massive hydrofluoric acid production. In this application note, fluorine content in coal is determined by ion chromatography after pyrohydrolysis.

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/DIS 18127.

Organic halides must be monitored in the environment. Combustion ion chromatography (CIC) is used for accurate halogen analysis in solids following EN 17813:2023.

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.