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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.

The Restriction of Hazardous Substances (RoHS) Directive 2002/95/EC stipulates maximum limits for the hazardous metals cadmium, lead and mercury as well as the hexavalent chromium and the brominated flame retardants in electrical and electronic products. To ensure compliance, reliable analysis methods are required.This poster deals with the wet-chemical determination of trace concentrations of the six RoHS-restricted substances in a wide variety of materials including metals, electrotechnical components, plastics and wires. After sample preparation according to IEC 62321, the metals lead, cadmium and mercury are best determined by anodic stripping voltammetry (ASV) and the flame retardants PBB and PBDE are quantified by direct-injection ion chromatography (IC) using spectrophotometric detection. Chromium(VI) can be determined either by adsorptive stripping voltammetry (AdSV) or IC. Both methods are very sensitive and meet prescribed RoHS limits.

Determination of chloride and sulfate in the presence of high nitrate concentrations. Optimization of the chromatographic separation by variation of the temperature and eluent composition.

The determination of cyanide is very important not only in electroplating baths and when decontaminating wastewater but, due to its high toxicity, also in water samples in general. Concentrations of 0.05 mg/L CN- can already be lethal for fish.This Bulletin describes the determination of cyanide in samples of different concentrations by potentiometric titration.Chemical reactions:2 CN- + Ag+ → [Ag(CN)2]-[Ag(CN)2]- + Ag+ → 2 AgCN

This Application Bulletin gives an overview of the volumetric 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 E203.

This Bulletin describes fluoride determination in various matrices with the help of the ion-selective fluoride electrode (F-ISE). The F-ISE is comprised of a lanthanum fluoride crystal and exhibits a response in accordance with the Nernst equation across a wide range of fluoride concentrations.The first part of this Bulletin contains notes regarding the handling and care of the electrode and the actual fluoride determination itself. The second part demonstrates the direct determination of fluoride with the standard addition technique in table salt, toothpaste and mouthwash.

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;

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.

The metals Cd, Co, Cu, Fe, Ni, Pb, and Zn are determined in the sub-ppb range (limit of detection 0.05 µg/L) by means of stripping voltammetry. The DP-ASV method is used for Cd, Cu, Pb, and Zn whereas Co, Ni, and Fe are determined by means of the DP-CSV method (dimethylglyoxime or catechol complexes).Use of the VA Processor and the sample changer allows automatic determination of the above metal ions in one solution. The method has been specially developed for trace analysis in the manufacture of semiconductor chips based on silicon. It can naturally also be employed successfully in environmental analysis.

The determination of the physical and chemical parameters as electrical conductivity, pH value, p and m value (alkalinity), chloride content, the calcium and magnesium hardness, the total hardness, as well as fluoride content are necessary for evaluating the water quality. This bulletin describes how to determine the above mentioned parameters in a single analytical run.Further important parameters in water analysis are the permanganate index (PMI) and the chemical oxygen deman (COD). Therefore, this Bulletin additionally describes the fully automated determination of the PMI according to EN ISO 8467 as well as the determination of the COD according to DIN 38409-44.

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 describes the simultaneous potentiometric titration of free boric acid and free tetrafluoroboric acid in nickel plating baths. After addition of mannitol, the formed mannitol complexes are titrated with sodium hydroxide solution. The determination is carried out directly in the plating bath sample; nickel and other metal ions do not interfere.

The standard method postulated by DIN 38406 Part 16 describes the determination of Zn, Cd, Pb, Cu, Tl, Ni, and Co in drinking, ground, surface and precipitation (e.g. rain) water. Because the presence of organic substances in the water samples can strongly interfere with the voltammetric determination, a pretreatment with UV digestion using hydrogen peroxide is necessary. This digestion ensures the elimination of all organic substances without introduction of blank values. These methods can, of course, also be applied for trace analysis in other materials, e.g. trace analysis in the production of semiconductor chips based on silicon. Zn, Cd, Pb, Cu, and Tl are determined on the HMDE by means of anodic stripping voltammetry (ASV), Ni and Co by means of adsorptive stripping voltammetry (AdSV).

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.

Cleanliness is indispensable in electronics production. Ionic contaminations in particular lead to a drastic worsening of the quality of the printed circuit boards. The present Application Note describes the determination of cations on printed circuit board surfaces. The intelligent Partial Loop Injection Technique (MiPT) used for this purpose permits the determination of cations and anions in the same sample. The determination of the anions is described in AN-S-317.

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.

This Application Note describes the determination of N,N-diethylhydroxylamine (DEHA), triisopropanolamine (TIPA) and a cationic color developing component (CDC) in a developer solution. The analysis is performed on a high-capacity column such as Metrosep C - 250/4.0 with subsequent direct conductivity detection. To reduce the residence time of the strongly retained color developer components, the column flow rate is increased after the elution of the amines.

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 EU directive for limiting the use of certain hazardous substances in electrical and electronic devices and IEC 61249-2-21 define limit values for halogen contents in materials that are used in electronics. Metrohm Combustion IC with ion chromatography determination permits precise, rapid and automated halogen determination in raw materials that are used in printed circuit boards according to IEC 61189-2.Keyword: pyrohydrolysis

Hydrogen peroxide is available in different purity grades depending on its use. High purity H2O2 (electronic grade) requires very low contamination levels, e.g., less than 1 μg/L of trimethylamine (TMA). This application describes the determination of trimethylamine in a high-purity H2O2 solution (30%). Analysis is performed using Inline Preconcentration with Matrix Elimination (MiPCT-ME) applying conductivity detection after sequential cation suppression.

Trace cation analysis in high purity water (sub-μg/L range) requires cation chromatography after sequential suppression and intelligent Preconcentration Technique (MiPCT). Trace cations in deionized water (DI) are determined and the method detection limit (MDL according to US EPA) as well as the limit of detection (LOD = 3 x S/N) is calculated. MDL and LOD are very similar in the lowest ng/L range for this setup with 6 mL preconcentration volume.

Cation analysis by IC in wastewater is a proven method. Limiting factor is often the Na/NH4 separation. High sodium concentrations may make ammonium determination impossible due to peak overlapping. The use of sequential suppression and a Dose-in gradient improve the Na/NH4 separation and enables determination of low ammonium concentrations.

Determination of trace levels of cations and amines in hydrogen peroxide is important in quality determination of high-grade semiconductor chemicals. In particular, some manufactures look for 1 ppb trimethylamine or less in hydrogen peroxide samples. Ion chromatography after MiPCT-ME* with conductivity detection after sequential cation suppression is applied.

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.

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.

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 determination of heavy metal ions in a solution is one of the most successful application of electrochemistry. In this application note, anodic stripping voltammetry is used to measure the presence of two analytes, in a sample of tap water.

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).

Capacitors are electronic components necessary for the success of the electronics industry. They have also become essential components of both electric and hybrid vehicles. Electrochemical tests, such as potentiostatic cyclic voltammetry, are used to check the performance of capacitors. VIONIC powered by INTELLO can perform both staircase and linear cyclic voltammetries (CV). This Application Note gives a comparison between the linear and the staircase potentiostatic cyclic voltammetries and highlights the necessity of using the linear CV to best study the performance of capacitors.

In this Application Note, hydrogen permeation experiments are conducted following the procedure described in the ASTM standard G148.

The Devanathan-Stachurski cell (or «H cell») is successfully used to evaluate the permeation of hydrogen through sheets or membranes. As small amounts of hydrogen pass through the sheet or membrane, a very sensitive potentiostat is required for its detection. A study of the hydrogen permeation properties of different iron sheets is discussed in this Application Note while taking the instrumental requirements into account.

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.

Electrochemical impedance spectroscopy (EIS) is a powerful technique which provides information about the processes occurring at the electrode-electrolyte interface. The data collected with EIS are modeled with a suitable electrical equivalent circuit. The fitting procedure will change the values of the parameters until the mathematical function matches the experimental data within a certain margin of error. In this Application Note, some suggestions are given in order to get acceptable initial parameters and to perform an accurate fitting.

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

This Application Note explains how fluoride determination in acid etching baths can be performed with thermometric titration.

Determination of mixtures of phosphoric, nitric, and acetic acids used in etching aluminum in the manufacture of semiconductor devices.

Determination of bromide and chloride in photographic developer solutions.

Determination of hydrofluoric acid in mixed acid etchant solutions.

Automated determination of the H2SiF6 and HF contents of industrial grade hexafluorosilicic acid.

This Application Note describes the determination of fluoride in silicon etch solutions with thermometric titration.

Determination of concentrated potassium hydroxide solutions which had been used for the etching of substrates containing silicon.

Determination of the total acids concentration in mixtures of nitric-hydrofluoric acid intended for etching silicon substrates.

Two separate titration sequences are required to analyze the mixture:- titration of the HF content with Al(NO3)3 (the «elpasolite» reaction)- titration of the H2SO4 with BaCl2 followed by titration with NaOH to determine the «total acids» contentThe HF, H2SO4, and «total acids» contents are converted to a HNO3 equivalent, with the HNO3 content found by subtracting the HF and H2SO4 from the «total acids» content.

Thermometric titration can be used for the ready determination of sulfuric acid and phosphoric acid in acid mixtures. An endpoint for each acid appears on the titration curve that can be used to quantify the respective acid.

Thermometric titration is used for the determination of hydrochloric acid and phosphoric acid in acid mixtures. Two endpoints appear on the titration curve that are used for the determination of the two acids.