Aplikace

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).

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.

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.

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.

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.

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

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 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 is used to determine hydrofluoric acid and nitric acid in etching baths containing ethanol and acetonitrile. Two endpoints appear on the titration curve that are used individually for the quantification of the respective acid.

Following the addition of caustic soda, hexafluorosilic acid can be determined through back titration of excess hydroxide with hydrochloric acid. Hydrofluoric acid (hydrogen fluoride) is determined by precipitation with aluminum in the presence of sodium and potassium ions. Nitric acid is determined by subtracting the equivalence concentrations of hexafluorosilic acid and hydrofluoric acid from the total acid concentration.

Nitric acid, phosphoric acid, and acetic acid are easily determined in etching baths using thermometric titration (TET). Compared to potentiometric titration, TET is faster and more convenient. Analysis is complete in less than two minutes.

Cyanides are used in some industrial processes, but if not handled carefully, they could contaminate the wastewater. In an acidic or neutral environment, this contaminated wastewater can form highly toxic hydrogen cyanide gas. Furthermore, the cyanide salts could also poison the environment and enter the ground water system. Therefore, it is essential to monitor the content of cyanide in effluent water. Cyanides can be easily determined with a cyanide ion-selective electrode. This application note presents a method for cyanide analysis according to APHA Method 4500-CN and ASTM D2036.

Determination of anions in solder paste after alcoholic extraction using anion chromatography with direct conductivity detection.

Determination of silica (as silicate) in pure water with preconcentration using anion chromatography with direct conductivity detection (without any post-column reaction).

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

In the semiconductor industry, thermoset resins combined with fabric or paper are used as an intermediate layer between substrates of printed circuit boards (PCB). These polymer-based sheets (laminates) are chosen depending on thickness and their thermomechanical and electrical characteristics. Near infrared spectroscopy (NIRS) is a fast, non-destructive and easy-to-use analytical method which allows the measurement of multiple key quality parameters in less than a minute. The following Application Note describes the determination of the transition time of PCB laminates by NIRS, a parameter correlating with the thickness, glass transition temperature, and tensile strength of the material.

Fast and reliable detection of phosphoric, sulfuric, nitric, and hydrofluoric acids with near-infrared spectroscopy in under one minute.

This application note discusses an alternative near-infrared (NIR) spectroscopy method that can reliably determine all parameters within a minute, even in complex acid mixtures.

Determination of citrate, ascorbate, and acetate in photographic developer solution using ion-exclusion chromatography with suppressed conductivity detection.

Cyanide in wastewater is an important parameter to measure for health requirements. Free, weakly complexed, and strongly complexed cyanide can be differentiated. Direct measurement in the wastewater is not feasible due to the matrix itself. Therefore, total cyanide is determined after acidification of the sample, which releases all cyanide from complexes, and subsequent distillation and absorption of cyanide in an alkaline solution. Amperometric detection is applied using a gold working electrode. This electrode is advantageous over the silver electrode due to less contamination issues and better long-term stability.

In an electroless plating bath, the consumed ingredients have to be regularly replenished to ensure an even layer of nickel-phosphorus alloy. This requires online monitoring of the active bath constituents. Parameters to be controlled are pH value (4.5–5.0) as well as nickel (NiSO4 < 10 g/L) and hypophosphite concentration (NaH2PO2: 1–12%). Other measurement options include sulfate, alkalinity, and organic additives (via CVS).

The chemicals used in the manufacture of semiconductors must exhibit an exceptional purity, because even traces of contaminants have a negative effect on electrical properties. For the manufacture of printed circuit boards, the light-sensitive photoresist applied to the substrate (wafer) is exposed to light at defined areas with the aid of a photo template and then developed in a chemical reaction. The developer contains 2.38 to 2.62% tetramethylammonium hydroxide (TMAH) and ensures that the exposed areas can be readily separated from the substrate. The monitoring of the TMAH concentration in the developer solution takes place with a process analyzer from Metrohm Applikon that is configured specially for titration. In addition to this, the analyzer helps with the mixing of the TMAH solutions.

The planarity and smoothness of silicon wafers are fundamental to manufacture optimal semiconductor devices, and Chemical Mechanical Planarization (CMP) is the most common technology used to achieve ultra-flat surfaces. A slurry is used for this purpose, composed of deionized water, a colloidal silicon or alumina liquid dispersion, and hydrogen peroxide, which has to be constantly monitored at all times.Online monitoring of the CMP process is necessary to avoid chemical waste and enhance wafer production yields. Metrohm Process Analytics can measure not only the H2O2 concentration, but also pH, conductivity, and temperature using the multipurpose 2060 Process Analyzer.