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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 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.

Thermometric titration is used for the determination of hydrochloric acid and nitric acid in acid baths. The entire acid content is titrated with caustic soda in the initial titration; the hydrochloric acid content is then determined in a second titration using silver nitrate solution.

Thermometric titration is used to determine hydrochloric acid and hydrofluoric acid (hydrogen fluoride) 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.

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.

Determination of nitrate in a copper plating bath after conversion of nitrate to ammonium. Direct potentiometric measurement using the NH3-ISE.

Determination of fluoride in a chromium plating bath by direct potentiometry using the F-ISE.

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.

Rapid inline monitoring of the major SC1/SC2 bath constituents is possible with reagent-free near-infrared spectroscopy, e.g., the 2060 The NIR-R Analyzer.

Lithium is a soft alkali metal that is typically obtained from salt lake brines. Lithium is used for many applications, but especially for production of lithium-ion batteries in electric cars, mobile phones, and more. This Process Application Note presents a method to monitor lithium as well as other cations in brines by online process ion chromatography (IC), a multiparameter analytical technique that can measure ionic analytes in a wide range of concentrations.

Etching is a vital process in semiconductor fabrication, involving the chemical removal of layers from the wafer substrate. Strict quality control measures are necessary to determine acid etchant concentrations in mixed acid solutions (e.g., SPM, DSP, or DSP+), critical for optimizing etch rate, selectivity, and uniformity during multiple wafer etching steps. This application presents a method to measure sulfuric acid and hydrogen peroxide in etching baths simultaneously using Raman spectroscopy with the PTRam Analyzer from Metrohm Process Analytics.

Monitoring organic additives in copper plating baths is crucial. The 2060 CVS Process Analyzer optimizes copper electroplating by providing precise bath control.

Determination of fluoride, chloride, and nitrate in a solution of NiSO4, ZnSO4 in sulfuric acid using anion chromatography with conductivity detection after chemical suppression.

Determination of fluoride, nitrate, phosphate, and sulfate in an etching reagent using anion chromatography with conductivity detection after chemical suppression.

Determination of chloride, nitrate, and sulfate in ultrapure water after sample preconcentration using anion chromatography with conductivity detection after chemical suppression.

Determination of chloride, nitrate, bromide, and sulfate in process wastewater using anion chromatography with conductivity detection after chemical suppression.

Determination of fluoride, chloride, nitrate, phosphate, and sulfate in wastewater using anion chromatography with conductivity detection after chemical suppression.

Determination of bromoacetate, methanesulfonate, chloride, phosphate, and sulfate in an acidic cleaning solution using anion chromatography with conductivity detection and chemical suppression.

Determination of bromide, sulfite, sulfate, and thiosulfate in a photographic developer solution using anion chromatography with conductivity detection after chemical suppression.

Determination of fluoride, acetate, formate, chloride, nitrite, nitrate, phosphate, and sulfate in wastewater containing N-methylpyrrolidone using anion chromatography with conductivity detection after chemical suppression and inline matrix elimination.

Determination of formate, chloride, nitrate, phosphate, and sulfate in 20% TMAOH using anion chromatography with conductivity detection after sequential suppression and inline matrix neutralization.

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 anions 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 cations is described in AN-C-149.

Electronic-grade nitric acid may not contain more than the slightest traces of anion contaminations (in the mg/L range). The ion chromatography determination of these kinds of anion traces requires not only a high-capacity column but also an eluent that allows the nitrate to be eluted by the column, although only after all of the other ions of interest have been eluted. This separation is achieved on a column of the Metrosep A Supp 16 - 250/4.0 type with the aid of a strong carbonate/hydrogen carbonate eluent.

Pyrophosphate is used as a stabilizer in aqueous hydrogen peroxide solution. “Reagent grade” solutions may contain pyrophosphate in the higher mg/L range, while “electronic grade” hydrogen peroxide should be free of this stabilizer. Here the determination of pyrophosphate in a high purity H2O2 solution (30%) is performed applying Inline Preconcentration with Matrix Elimination (MiPCT-ME) and a Dose-in Gradient.

The microbore Metrosep A Supp 4 - 250/2.0 column is particularly suitable for the analysis of anions in critical samples. A waste water sample is being analyzed in the current application. The sample requires only one filtration prior to injection on the Metrosep A Supp 4 - 250/2.0. The anions are quantified with the application of conductivity detection following sequential suppression.

Ultrapure chemicals are required in the semiconductor industry. Ionic impurities may lead to compromised products. This application describes the determination of anionic impurities in semiconductor grade 28% ammonium hydroxide solution. To avoid matrix disturbances, Inline Neutralization and Inline Preconcentration with Matrix Elimination needs to be applied.

The semiconductor industry requires high-purity or even ultrahigh-purity chemicals for the production of electronic components. The purity of the chemicals is crucial for the quality and efficient production of the parts. Here, hydrogen peroxide and ammonium hydroxide are analyzed applying traditional sample preparation methods like digestion and evaporation with subsequent reconstitution with ultrapure water. The received samples are injected applying intelligent Preconcentration Technique (MiPCT).

Determination of hydrofluoric and nitric acid in etching baths by potentiometric titration.a) Determination of the total acid content using the combined Sb electrode and NaOH as titrant.b) Determination of hydrofluoric acid using the F-ISE and the titrant La(NO3)3.The concentration of nitric acid is then determined by calculation.

Acid copper baths are mainly used for the copper deposition on semiconductor wafers. Small amounts of chloride increase the speed of deposition and reduce anode polarization. However, higher concentrations are undesired, as this will decrease the quality of the copper deposition. Therefore, it is quite important to monitor the amount of chloride to have an effective, yet high-quality copper deposition process.In this Application Note, a fully automated solution based on titration is presented. In comparison to ion chromatography, titration offers the benefit that no dilution of the sample is necessary, and the hardware is comparatively low-priced. Furthermore, the fully automated solution allows users to minimize handling errors, to reduce workloads, and to guarantee outstanding reproducibility.

Electroplating processes are used in several different industry sectors to protect the surface quality of various products against corrosion or abrasion and significantly improve their working life. It is essential to check the bath composition on a regular basis to ensure that the process is operating correctly. Typical examples of electroplating baths include alkaline degreasing baths or acidic or alkaline baths containing metals e.g. copper, nickel, or chromium, or components like chloride and cyanide. It is crucial that the chosen analysis technique fulfills high safety standards for these kinds of analyses and produces reliable results. The OMNIS Sample Robot system automatically pipettes and analyzes aggressive electroplating bath samples on different workstations, increasing the safety in the lab. This provides more reliable results in comparison to manual titration and is more time efficient as different parameters can be analyzed in parallel.

Boehm titration is a quantitative analysis of functional groups on the surface of carbon materials based on their reactions with basic solutions of NaHCO3 (pKa = 6.4), Na2CO3 (pKa = 10.3), and NaOH (pKa = 15.7). This is a cost-efficient method that gives absolute values with high precision of the accessible, mainly oxygen-containing functional groups on the surface. Originally, Boehm titration was developed for carbon materials like conductive carbon black (CCB), activated carbon, porous carbon, and graphite. Modern carbon-based materials like graphene, graphene oxide (GO), or carbon nanotubes can also be analyzed this way.

This Application Note compares the OMNIS Titrator and 888 Titrando for determinations of nitric acid, phosphoric acid, and acetic acid in an aluminum etching bath, as well as the determination of tetramethylammonium hydroxide (TMAH). Identical analysis parameters were used, showing that OMNIS delivers results on par or even better than with other established titration systems.

The pH value in carbon black, an essential additive in modern lithium-ion batteries, is accurately and reliably analyzed in this Application Note by using the 913 pH Meter equipped with a Unitrode easyClean according to ASTM D1512 as well as ISO 787-9 and GB/T 1717-1986.

Determination of silicate and hexafluorosilicate (calculated) using anion chromatography with conductivity detection after chemical suppression (see AN S-277) and subsequent UV/VIS detection with post-column reaction. Hexafluorosilicate is hydrolyzed into fluoride and silicate. Both anion concentrations may be used for the calculation of the SiF62- concentration.

Simultaneous determination of Zn, Cd, Pb, Cu, Fe, Ni, and Co in 50% NaOH.

Lead is commonly used as stabilizer in electroless nickel plating processes. The regular and precise determination of the electrochemically active Pb(II) concentration is essential to keep the plating process running optimally under stable conditions. Differential pulse anodic stripping voltammetry can be used to determine the active lead content after dilution. The voltammetric determination has been established as a straightforward, sensitive, selective, and interference-free method for this application.

Determination of Zn, Cd, Pb, Ni, and Co in hydrochloric acid (37.8%).

Determination of Zn, Cd, Pb, Ni, and Co in Javelle water.

Determination of Zn, Cd, Pb, Ni, and Co in FeCl3 solution of 40%.

The concentration of Fe is determined polarographically in phosphoric acid. The method is suitable for iron in concentrations in the ppm range. Fe(II) and Fe(III) show signals with the same sensitivity

The concentration of Ni and Co is determined by adsorptive stripping voltammetry at the HMDE with dimethylglyoxime (DMG) as complexing agent.

The concentration of Fe is determined by adsorptive stripping voltammetry at the HMDE with 1-nitroso-2-naphthol (1N2N) as complexing agent.

Determination of suppressor «Copper GleamTM 2001 Carrier» in acid copper baths by dilution titration (DT) using cyclic voltammetric stripping (CVS).

Determination of brightener «Copper GleamTM 2001 Additive» in acid copper baths by modified linear approximation technique (MLAT) using cyclic voltammetric stripping (CVS).

Determination of suppressor «Cupracid BL-CT» in acid copper baths by dilution titration (DT) using cyclic voltammetric stripping (CVS).

Determination of brightener «Cupracid BL» in acid copper baths by linear approximation technique (LAT) using cyclicvoltammetric stripping (CVS).

Determination of suppressor «Cupraspeed» in acid copper baths by dilution titration (DT) using cyclic voltammetric stripping (CVS).

Determination of brightener «Cupraspeed» in acid copper baths by modified linear approximation technique (MLAT)using cyclic voltammetric stripping (CVS).

Determination of suppressor «MACuSpecTM PPR 100 Wetter» in acid copper baths by dilution titration (DT) using cyclic voltammetric stripping (CVS).

Determination of brightener «MACuSpecTM PPR 100 Brightener» in acid copper baths by modified linear approximation technique (MLAT) using cyclic voltammetric stripping (CVS).

Determination of suppressor «MultiBondTM 100 Part A20» in an acid copper bath by dilution titration (DT) using cyclicvoltammetric stripping (CVS).

Determination of suppressor «Ronastan TP Additive» in a tin/lead bath by dilution titration (DT) using cyclic voltammetric stripping (CVS).

Determination of suppressor «Solderon ST-200 Primary» in a tin bath by dilution titration (DT) using cyclic voltammetric stripping (CVS).

Determination of suppressor «InPulse H6» in acid copper baths by dilution titration (DT) using cyclic voltammetric stripping (CVS).

Determination of brightener «InPulse H6» in acid copper baths by modified linear approximation technique (MLAT) using cyclic pulse voltammetric stripping (CPVS).

The concentration of Ni in a Ni plating bath is determined by polarography in ammonia buffer pH 9.6.

The concentration of Sb(III) and Sb(total) in an electroless nickel bath is determined by anodic stripping voltammetry (ASV). In c(HCl) = 0.6 mol/L only Sb(III) shows a signal. In w(HCl) = 10% the Sb(total) content is determined.

Determination of suppressor «Thru-Cup EVF-B» in acid copper baths by dilution titration (DT) using cyclic voltammetric stripping (CVS).

Determination of brightener «Thru-Cup EVF-1A» in acid copper baths by modified linear approximation technique (MLAT) using cyclic voltammetric stripping (CVS).

Determination of leveler «Thru-Cup EVF-R» in acid copper baths by response curve technique (RC) using cyclic voltammetric stripping (CVS).

The concentration of Pd in an activator bath is determined by polarography in ammonium chloride electrolyte.

Determination of suppressor «Top Lucina α-M» in acid copper baths by dilution titration (DT) using cyclic voltammetric stripping (CVS).

Determination of brightener «Top Lucina α-2» in acid copper baths by modified linear approximation technique (MLAT) using cyclic voltammetric stripping (CVS).

Determination of leveler «Top Lucina α-3» in acid copper baths by response curve technique (RC) using cyclic voltammetric stripping (CVS).

The EU directive on «Restriction of Hazardous Substances» (RoHS) requires the testing of four regulated heavy metals (Pb, Hg, Cd, Cr(VI)) in electrotechnical products. After sample preparation according to IEC 62321 the determination of lead and cadmium in electronic components can be carried out by anodic stripping voltammetry (ASV) using ammonium oxalate buffer pH 2.

The EU directive on «Restriction of Hazardous Substances» (RoHS) requires the testing of four regulated heavy metals (Pb, Hg, Cd, Cr(VI)) in electrotechnical products. After sample preparation according to IEC 62321 the determination of chromium(VI) in electronic components can be carried out by polarography in ammonia buffer pH 9.6.

The EU directive on «Restriction of Hazardous Substances» (RoHS) requires the testing of four regulated heavy metals (Pb, Hg, Cd, Cr(VI)) in electrotechnical products. After sample preparation according to IEC 62321 the determination of mercury in electronic components can be carried out by anodic stripping voltammetry (ASV) at a gold rotating disk electrode (Au-RDE).

The EU directive on «Restriction of Hazardous Substances» (RoHS) requires the testing of four regulated heavy metals (Pb, Hg, Cd, Cr(VI)) in electrotechnical products. After sample preparation according to IEC 62321 the determination of lead and cadmium in polymer materials can be carried out by anodic stripping voltammetry (ASV) using ammonium oxalate buffer pH 2.

The EU directive on «Restriction of Hazardous Substances» (RoHS) requires the testing of four regulated heavy metals (Pb, Hg, Cd, Cr(VI)) in electrotechnical products. After sample preparation according to IEC 62321 the determination of chromium(VI) in polymer materials can be carried out by polarography in ammonia buffer pH 9.6.

The EU directive on «Restriction of Hazardous Substances» (RoHS) requires the testing of four regulatedheavy metals (Pb, Hg, Cd, Cr(VI)) in electrotechnical products. After sample preparation according to IEC62321 the determination of mercury in polymer materials can be carried out by anodic stripping voltammetry (ASV)at a gold rotating disk electrode (Au-RDE).

The EU directive on «Restriction of Hazardous Substances» (RoHS) requires the testing of four regulated heavy metals (Pb, Hg, Cd, Cr(VI)) in electrotechnical products. After sample preparation according to IEC 62321 the determination of lead and cadmium in metallic materials can be carried out by anodic stripping voltammetry (ASV) using ammonium oxalate buffer pH 2.

The EU directive on «Restriction of Hazardous Substances» (RoHS) requires the testing of four regulated heavy metals (Pb, Hg, Cd, Cr(VI)) in electrotechnical products. After sample preparation according to IEC 62321 the determination of chromium(VI) in chromate coating on metallic materials can be carried out by adsorptive stripping voltammetry (AdSV) using DTPA (diethylenetriamine pentaacetic acid) as complexing agent.

The EU directive on «Restriction of Hazardous Substances» (RoHS) requires the testing of four regulated heavy metals (Pb, Hg, Cd, Cr(VI)) in electrotechnical products. After sample preparation according to IEC 62321 the determination of mercury in metallic materials can be carried out by anodic stripping voltammetry (ASV) at a gold rotating disk electrode (Au-RDE).

Electroless nickel plating is an important and well established process in the surface finishing industry. In the past, the addition of small amounts of lead has widely been used to stabilize the plating bath. With the increasing number of restrictions in recent years on the use of lead in consumber products, particularly electronics, alternative stabilizers were developed and introduced. One of the stabilizers used as lead replacement is iodate. It can be used as a single additive or in combination with bismuth or antimony. This method allows the determination of iodate directly in the plating bath sample by polarography. The method is simple and fast, however, sensitive and robust.

Electroless nickel plating is an important and well established process in the surface finishing industry. In the past the addition of small amounts of lead has widely been used to stabilize the plating bath. With the increasing number of restrictions in recent years on the use of lead in consumber products, particularly electronics, alternative stabilizers were developed and introduced. Two of the stabilizers used as lead replacement are antimony and bismuth. They can be used as a single additive or in combination with each other or iodate. This method allows the determination of antimony and bismuth directly in the plating bath sample by anodic stripping voltammetry (ASV). The method is simple and fast, however sensitive and robust

Controlling Au(I) levels in gold plating baths is required for high quality. Voltammetric analysis with the Multi-Mode Electrode Pro is an efficient solution.

Monitoring Sb(III) stabilizer levels during electroless Ni plating is critical for high-quality coatings. Anodic stripping voltammetry offers fast, reliable Sb(III) analysis.

Electroless nickel plating ensures low-cost wear and corrosion resistance. Monitoring lead stabilizer levels in Ni plating baths is possible with the Bi drop electrode.

Electroless Ni plating offers superior surface finish and corrosion resistance. Anodic stripping voltammetry allows Bi stabilizer to be monitored in Ni plating baths.

Raman spectroscopy at 532 nm excitation is used to study the crystalline and amorphous content of mixed phase silicon films.

This article describes the coupling of ion chromatography with mass spectrometry (IC-MS) and plasma mass spectrometry (IC-ICP/MS) for the trace analysis of potentially hazardous compounds in the environment.

The automated combination of pyrolysis and subsequent ion chromatography (Combustion IC) permits the parallel detection of halogens and sulfur in all flammable solid and liquid matrices. The method is captivating, not only because of its outstanding precision and trueness, but also because of the high sample throughput.

NIR spectroscopy has been traditionally limited due to the water absorption in this spectral range. In this way, the well-known water restriction has limited the development of new applications for NIR spectroelectrochemistry. In this work, several interesting alternatives are proposed in order to minimize or even to remove the aqueous contribution in this spectral range.

For the past three decades, Cyclic Voltammetric Stripping (CVS) has been the standard practice for analyzing organic additives in electroplating copper baths in the circuit board and wafer plating industries. The variations in the compositions of such baths have created a need for more optimized method development routines. New advancements in the hardware and software protocols for CVS have simplified the overall process of method optimization to a great extent. In this study, the process of method optimization is discussed in conjunction with these protocols.

The demand for microelectronics and printed circuit boards (PCBs) has steadily increased as more flat panel displays, LEDs, photovoltaics, and other essential intermediates are required to create modern consumer devices. This is favorable for the semiconductor industry, though challenges may arise to deliver on time while upholding high quality standards. To be successful, several processes must be optimized in order to increase production efficiency. This White Paper describes the capabilities of the modern analytical method near-infrared (NIR) spectroscopy for assessing the quality of acid baths for etching of microelectronics and printed electronics. Not only are analysis times sharply reduced to less than a minute, the related running costs are also significantly lower – certainly a boost in efficiency that should not be overlooked!

White paper about Raman spectroscopy and electrochemistry and their combination (electrochemical Raman).

This White Paper focuses on selected IC-MS applications for the straightforward identification and quantification of organic acids and inorganic anions in different matrices.

This White Paper discusses the concept and benefits of NIR spectroscopy and outlines several real-life laboratory application examples with the use of OMNIS NIRS, the cutting-edge NIR spectrometer from Metrohm.

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