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In this article portable Raman spectroscopy as an effective tool for at-line characterization of carbon black is presented. Raman spectroscopic analysis can be an effective test to characterize carbon black material, including the structural order.

The poster shows the use of Vis-NIR spectroscopy for the simultaneous quantification of cobalt content, solids content, relative density and viscosity in paint driers as an outstanding alternative to conventional wet chemical laboratory methods. The advantages of the expanded wavelength range over the visible range become clear in this application: the visible range (400 – 780 nm) correlates directly with the cobalt content; the NIR range (780 – 2500 nm) is used for determining the chemical and physical parameters.

Halides interfere with most determinations of mercury or silver. However, if mercury or silver is titrated with sulfide ions, extremely insoluble sulfides are formed.A simple method is described that allows the direct titration of mercury(II) or silver(I) compounds in the presence of halides. The potentiometric titration takes place under alkaline conditions using thioacetamide as the titrant after formation of the EDTA complex.Organic compounds that are insoluble in alkaline EDTA can also be titrated after a Schoeniger digestion.

Generally speaking, the gas extraction or oven method can be used for all samples which release their water when they are heated up. The oven method is indispensable in cases in which the direct volumetric or coulometric Karl Fischer titration is not possible, either because the sample contains disruptive components or because the consistency of the sample makes it very difficult or even impossible to transfer it into the titration vessel.The present Application Bulletin describes automatic water content determination with the aid of the oven technique and coulometric KF titration, using samples from the food, plastic, pharmaceutical and petrochemical industry.

Near-infrared spectroscopy is used for a wide range of analyses. Thanks to its fast and non-destructive determination, NIRS is outstandingly suited to quality control of products and raw materials, whether during production or on the finished product. This Application Bulletin shows NIR applications and feasibility studies from the lacquer and paint industry performed using NIRSystems devices.

Pyrithione complexes, such as zinc pyrithione (ZnPT), copper pyrithione (CuPT), and sodium pyrithione (NaPT), are used as fungicides and bactericides. ZnPT is used in the treatment of skin conditions such as seborrheic dermatitis or dandruff. Furthermore, ZnPT is sometimes used as an antibacterial agent in paints to prevent algae and mildew growth. CuPT is primarily in use as a biocide to prevent biofouling of surfaces submerged in water. Meanwhile, NaPT is used as antifungal agent for treatment of mycosis, such as athlete’s foot. The different pyrithione complexes are determined by iodometric titration using a maintenance-free Pt Titrode for the indication.

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.

Determination of bromide and chloride in photographic developer solutions.

In the synthesis of certain dyes, sodium chloride is a byproduct. The content of chloride is therefore an important parameter. This Application Note describes the determination of the chloride content in dye by standard addition using a Cl- ion-selective electrode.

Lucigenin is one of the most often used chemiluminescent reagents and might be used for e.g., the indication of the presence of superoxide anion radicals.Lucigenin is rather expensive to buy, however, its synthesis only includes a two stage synthesis starting from acridanone. The first stage includes an Nmethylation, the second forms the lucigenin chloride, which is finally transformed into lucigenin nitrate. To check the purity of the synthesized lucigenin, ion measurement can be applied using a nitrate selective electrode. This is a fast and inexpensive method compared to competing methods such as ion chromatography.

Acrylic dispersion paints are made of pigment suspended in acrylic polymer emulsions, which also include other organic material such as plasticizers, defoamers, or stabilizers. Acrylic dispersion paints are water-soluble but become resistant to water when dry. Due to the fact that once dry, acrylic dispersion paints can no longer be used, they should be stored air-tight at room temperature. For research purposes, it is of interest to assess the dissolved oxygen (DO) concentration in such samples as it is assumed that the DO amount can be related to the storage life. This Application Note describes a fast and accurate determination of dissolved oxygen by using an optical sensor.

Determination of water content in ink is possible with Karl Fischer titration, as shown in this Application Note.

The water content of color paste is determined according to Karl Fischer.

Chromate (Cr(VI)) is considered toxic and potentially carcinogenic, which is why its concentrations in children's toys should be kept as low as possible. The EU directive 2009/48/EC defines limit values for the migration of chromate from children's toys. The hydrochloric-acid-containing migration solution is diluted with a buffer. 2000 μL of this solution are injected automatically using intelligent preconcentration technology and matrix elimination. Detection takes place via ICP/MS.

Determination of chloride and sulfate in a reactive dye using anion chromatography with direct conductivity detection. Suppressed IC does not work as the dye is hydrolyzed in alkaline solution and releases sulfate.

This Application Note describes an NIR method for monitoring the esterification process in butyl acetate production. The developed NIR method shows excellent analytical performance equivalent to that obtainable with more time-consuming GC methods.

Ink is a complex mixture that, along with numerous additives, is comprised mainly of solvent, dye, water and surfactant. Vis-NIR spectroscopy is outstandingly suitable for providing rapid and reliable determinations of constituents in the context of quality controls. This Application Note describes the determination of diethylene glycol (DEG), water, dye and surfactant.

This Application Note shows the determination of two important additives – butylglycol and propylheptyl alcohol – in water-soluble lacquers using Vis-NIR spectroscopy. Other lacquer constituents can also be determined in addition to the two additives.

This Application Note shows how the amine number and the solids content in electrophoretic lacquer coatings can be determined quickly and simply with Vis-NIR spectroscopy. Additional parameters can be determined reliably and conveniently with a single measurement.

This Application Note describes the simultaneous determination of the four most important analysis parameters of paint dryers – cobalt and solids contents, specific weight and viscosity – using a VIS-NIR analyzer. The visible range correlates with the metal content, while the NIR region provides the specific weight, viscosity and solids content.

This Application Note shows that the visible range of the Metrohm Vis-NIR analyzer can be used to quantify the color intensity of dyes, providing comparable results to the reference analysis UV-Vis. The NIR region can be used in addition to distinguish between different dye types or different suppliers and can identify impurities in the undiluted dyes during raw material control. The combination of the visible and near-infrared wavelength ranges offer the benefit that only one analyzer is required to receive results on multiple parameters in a 30-seconds-scan results on both cost and time saving.

Packaging has become an indispensable part in the food manufacturing process. To improve the appearance and properties of the packaging, a wide variety of coatings and inks are used. Different additives enhance rheological properties, control the wetting dispersion, or in the case of wax increase abrasion resistance. The regulations of these coatings in food packaging applications are very strict in some countries, creating the need for close monitoring of the production process.A fast, reliable, and simple to use solution for quantifying rheological additives and wax in such coatings is Visible-Near Infrared Spectroscopy (Vis-NIRS). Both parameters are determined simultaneously by Vis-NIRS in less than a minute.

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

Solids used in road construction were analyzed with a hand-held Raman spectrometer. The materials examined are conventional pigments and resins, e.g., CaCO3, TiO2 and DEGALAN®. The measured spectra differ considerably from one another. In order to assess the main differences between the chemical structures, the peaks of the spectra were assigned to the functional groups that generated them.

Determination of chloride, sulfate, maleate, oxalate, and fumarate in ink using anion chromatography with conductivity detection after chemical suppression and dialysis for sample preparation.

Determination of chloride, phosphate, phosphite, and sulfate in a dye solution using anion chromatography with conductivity detection after chemical suppression.

Determination of fluoride, chloride, nitrite, bromide, nitrate, phosphate, sulfite, sulfate, and thiosulfate in colored liquors using anion chromatography with conductivity detection after chemical suppression.

Glycolate and lactate have to be determined in a dual phase varnish remover. Analyzed is only the upper aqueous phase. The separation is achieved on a Metrosep A Supp 16 - 250/4.0 column. The eluent composition is adapted to get a sufficient separation of glycolate and lactate without interference by formate and acetate. Conductivity detection after sequential suppression is applied.

Determination of the nitrogen content of nitrocellulose by potentiometric titration with Fe(II) using a combined Pt electrode.

The hydroxyl number is an important sum parameter for quantifying the presence of hydroxyl groups in a chemical substance. As a key quality parameter, it is regularly determined in various polymers like resins, paints, polyesterols, fats, and solvents. Unlike other standards, EN 4629-2 works pyridine-free and without refluxing at elevated temperatures for a longer time. The determination is based on the catalytic acetylation of the hydroxyl group. It is performed at room temperature, requires only a small sample volumen, and can be fully automated.This Application Note describes the potentiometric determination of the hydroxyl number in 1-octanol and polyethylene glycol according to EN 4629-2. Using the OMNIS DIS-Cover technique, all sample preparation steps can be fully automated. Furthermore, the use of an OMNIS Sample Robot allows parallel analysis of multiple samples. The average time per analysis for one sample is thus reduced from approximately 49 min to 25 min., considerably increasing productivity in the laboratory.

Dye samples are analyzed for trace chromate. Chromate (Cr(VI)) is considered toxic and potentially carcinogenic for which reason its concentrations should be as low as possible. This sample is prepared with C18 cartridges and injected applying Metrohm intelligent Preconcentration Technique (MiPCT). After each injection, the preconcentration column requires additional rinsing to eliminate matrix effects. For this purpose, no other instrument than an 800 Dosino is required. The system is optimized for sample volumes between 20 and 2000 µL. For most samples additional rinsing of the preconcentration column is not required.

Determination of Fe, Pb, Cd, and Cu in Co(Ac)2 solution using the MME.

More strict regulations paired with more complex products have increased testing complexity in the paint and coating industry. Therefore, producers ask for more powerful, safe and sustainable analytical methods. Testing by Vis-NIR spectroscopy is a sustainable and costefficient alternative to many wet chemical methods. This white paper describes how Vis-NIR spectroscopy improves testing procedures for various analyses during the formulation and production of paint and coatings in an economic and ecological way.Key words: testing, sustainable, VOC, paint, coating, binders, resins, additives, pigments, solvents

It is widely accepted that prolonged exposure to hexavalent chromium compounds can have dire health effects. This has led to increased regulation of chromium-containing products and greater demand for technologies that can positively identify hexavalent chromium in potential matrices. These include paints, dyes, and primers, which can pose a problem for interrogation with Raman, as strongly colored materials often exhibit fluorescence when stimulated at 785 nm. Fluorescence can obscure the Raman signal and prevent positive identification. MIRA XTR DS provides all the functionality of handheld material ID with a new capability that selectively eXTRacts the Raman signal from fluorescent materials. Fluorescence rejection at 785 nm provides higher sensitivity and resolution than 1064 nm systems, as well as a much wider scope of applications amenable to Raman spectroscopy. MIRA XTR DS offers a comprehensive and versatile material ID test solution for field operations.

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