Aplikace

The coupling of highly efficient ion chromatography (IC) to multi-dimensional detectors such as a mass spectrometer (MS) or an inductively coupled plasma mass spectrometer (ICP/MS) significantly increases sensitivity while simultaneously reducing possible matrix interference to the absolute minimum. By means of IC/MS several oxyhalides such as bromate and perchlorate can be detected in the sub-ppb range. Additionally, organic acids can be precisely quantified through mass-based determination even in the presence of high salt matrices. By means of IC-ICP/MS different valence states of the potentially hazardous chromium, arsenic and selenium in the form of inorganic and organic species can be sensitively and unambiguously identified in one single run.

The analytical challenge treated by the present work consists in detecting sub-ppm quantities of bromide, sulfate, aliphatic monocarboxylic acids and several alkaline earth metals in the presence of very high concentrations of sodium and chloride. Bromide, sulfate, acetate and butyrate can be reliably determined by suppressed conductivity detection. Due to matrix effects, propionate can only be detected qualitatively. This drawback can be overcome by coupling the ion chromatograph (IC) to a mass spectrometric (MS) detector. This results in reduced matrix interferences and significantly enhanced sensitivities. The cations magnesium, barium and strontium are determined by non-suppressed conductivity detection.

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

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

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

This Application Bulletin describes the determination of mercury by anodic stripping voltammetry (ASV) at the rotating gold electrode. With a deposition time of 90 s, the calibration curve is linear from 0.4 to 15 μg/L; the limit of quantification is 0.4 μg/L.The method has primarily been drawn up for investigating water samples. After appropriate digestion, the determination of mercury is possible even in samples with a high load of organic substances (wastewater, food and semi-luxuries, biological fluids, pharmaceuticals).

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

Copper is one of the few metals which is available in nature also in its metallic form. This and the fact that it is rather easy to smelt led to intense use of this metal already in the so-called Copper and Bronze Age. Nowadays, it is more important than ever, because of its good electrical conductivity and its other physical properties. For plants and animals, it is an essential trace element; for bacteria, in contrast, it is highly toxic.This Application Bulletin describes the determination of copper by anodic stripping voltammetry (ASV) using the scTRACE Gold electrode. With a deposition time of 30 s, the limit of detection is about 0.5 μg/L.

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

AOF (adsorbable organic fluorine) is used to screen for per- and polyfluorinated alkyl substances in aqueous matrices via pyrohydrolytic combustion and ion chromatography.

Combustion ion chromatography (CIC) measures AOX (adsorbable organically bound halogens, i.e., AOCl, AOBr, AOI) and AOF as well as CIC AOX(Cl) according to DIN 38409-59 and ISO/DIS 18127.

Tafel analysis is an important electrochemical technique used to understand reaction kinetics. By studying the Tafel slope, it reveals the rate-determining steps in electrode reactions, aiding fields like corrosion and fuel cell research. This method helps industries optimize processes and improve device performance by tailoring materials and conditions for greater efficiency.

Determination of ferrous ions in heat exchanger and vessel acid wash solutions, for measuring the effectiveness of acid inhibitors used in the solutions. Depending on the condition of the sample, the lower practical limit for the determination will vary from approximately 20-100mg/Kg Fe2+. Samples with high silicic acid contents require relatively large amounts of dilution water to render them mobile, and this limits the aliquot size and hence the amount of Fe2+ which can be analyzed.

Determination of chromium in leather waste solutions in the range between 1000 and 30,000 ppm.

Determination of calcium and magnesium in process solutions.

Determination of acetic, propionic, butyric, valeric, and caproic acid in produced water using anion chromatography with conductivity and MS detection after post-column addition of ammonia for MS detection and inline sample preparation by dialysis.

Determination of phosphate in produced water containing up to 100 g/L chloride as well as crude oil using anion chromatography with conductivity and MS detection after inline dialysis.

Determination of perchlorate in process water using anion chromatography with direct conductivity detection.

Determination of glycolic acid, formic acid, acetic acid and carbonic acid in a scrubber solution using ion-exclusion chromatography with conductivity detection after chemical suppression.

Determination of boric acid and acetic acid in process water using ion-exclusion chromatography with conductivity detection after chemical suppression.

Determination of glycolic acid, formic acid, glutaric acid, acetic acid, propionic acid, and butyric acid in paper industry process water using ion-exclusion chromatography with suppressed conductivity detection.

Determination of acetate and formate in an amine solution using anion chromatography with conductivity detection after suppression.

To optimize the wet-spinning process in the viscose/rayon production, it is crucial to measure sulfuric acid and zinc. H2SO4 and ZnSO4 are analyzed using a potentiometric titration and colorimetric measurement technique. Results are automatically validated against a known standard solution to guarantee preset control limits.

Boric acid requires precise monitoring in the primary circuit to control nuclear reactor reactivity. The 2060 TI Process Analyzer monitors boric acid online in near-real time.

This Process Application Note deals with the online monitoring of calcium and sulfate in flue gas scrubbing solutions using titration. Other contaminants that can be measured are sulfite, chloride, and chlorine. Low concentrations of heavy metals such as cadmium, zinc, copper, and lead can be measured in the ppb/ppm range with the ADI 2045VA Process Analyzer using voltammetry.

Strict rules governing hygiene apply in the food and beverage industry. All surfaces of materials that come into contact with foods or beverages must be disinfected in order to ensure their bacteriological purity. Peracetic acid (PES) is often used for rapid disinfection of PET bottles. Correct dosing of the acid must be observed while doing so: Too much PES impairs taste and causes unnecessary costs through increased consumption. Insufficient concentrations on the other hand are unable to guarantee satisfactory cleaning. The PES concentration can be determined exactly using a process analyzer specially configured for photometric analyses. The analyzer sends an alarm signal to the control system if the concentration should deviate from the specifications.

Beer is a popular beverage consumed by millions of people for enjoyment, despite its humble beginnings as a water purification technique in pre-modern times. Brewing beer requires large amounts of water which must adhere to strict alkalinity, hardness, and pH parameters to ensure uniformity in flavor and appearance between each batch. Alkalinity is introduced by carbonates and hydroxides in water which raise and buffer the pH. Hardness, balanced to a large degree by the alkalinity, comes from Ca and Mg ions, mainly present as hydrogen carbonates. Depending on the concentration ranges, the 2035 Process Analyzer or the 2060 Process Analyzer are ideally suited for the fully automatic execution of these important analyses, as well as additional parameters like pH or conductivity. These process analyzers can signal the plant’s distribution system to correct the water chemistry, ensuring consistent product quality. In addition to alkalinity and water hardness, numerous other parameters can also be determined (pH, conductivity, etc.).

In power plants, corrosion is the greatest enemy. If corrosive impurities are present in the circuit streams (e.g., chlorides and hydroxides), deposition of an insulating layer of scale on the heat transfer surfaces occurs, resulting in costly and critical downtimes. To ensure high throughput of power plants, online analysis of critical parameters such as sodium is highly advantageous for safety, protection, and process optimization. With the 2035 Process Analyzer from Metrohm Process Analytics, operators gain the information they need to accurately identify trends, reduce downtimes, and address operational issues before costly problems arise.

Determination of iodide and thiosulfate in photographic process wastewater using anion chromatography with amperometric detection at the carbon paste electrode after chemical suppression.

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

Determination of chloride, bromide, nitrate, sulfite, sulfate, phosphate, oxalate, thiosulfate, and thiocyanate (heat stable salts) in scrubber solutions using anion chromatography with conductivity detection after chemical suppression.

Determination of chloride, bromide, nitrate, sulfite, sulfate, oxalate, and thiosulfate in a process water of the paper industry using anion chromatography with conductivity detection after chemical suppression.

Determination of hypophosphite, phosphite, and phosphate in the presence of fluoride, chloride, and sulfate in process water using anion chromatography with suppressed conductivity detection.

Determination of chloride, sulfite, sulfate, and thiosulfate in a process water using anion chromatography with conductivity detection after chemical suppression and subsequent UV/VIS detection.

Determination of fluoride, acetate, propionate, formate, butyrate, chloride, nitrite, bromide, nitrate, benzoate, phosphate, sulfate, malonate, and oxalate in an industrial process water using anion chromatography with conductivity detection after sequential suppression.

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

ASTM D8234 describes the determination of anions in high saline water by applying suppressed conductivity followed by UV/VIS detection. This combination enables the determination of e.g. nitrite by UV detection. With conductivity detection, this quantification is not possible or difficult due to the very large chloride peak. The actual sample is a refining process liquid with a high chloride content. As the sample solution also contains organic material, Inline Dialysis is applied to protect the analytical column. The combination of the two detection modes and the Inline Dialysis option reduces manual sample preparation and substantially increases the accuracy of the analysis.

Process water from flue gas desulfurization mainly contains sulfite and sulfate. Besides these two main components, other sulfur species may be formed in the process. This application describes the determination of such late-eluting sulfur species with ion chromatography applying a Dose-in gradient. The applied gradient profile enables the resolution of amidosulfonate, dithionate, and imidodisulfonate besides thiosulfate, thiocyanate, major anions, and acetate.

Water hardness is often determined photometrically using two different indicators and while performing the determination at two different pH values. Additionally, the determination itself is subjective, as the color change is determined by the analyst and not by an analytical device.This application note introduces a more robust option to easily assess calcium, magnesium, and total hardness in water by using the Cu-ISE and two different titrants. Sample preparation is identical for both analyses and can therefore be automated without any issues.

Determination of sulfide and thiosulfate in a process water using anion chromatography with UV/VIS detection after chemical suppression and conductivity detection.

Determination of arsenite and arsenate in process water using ion-exclusion chromatography with UV detection.

Feedwater for steam generation in boiling water reactors (BWR) needs to be analyzed for corrosion products. Presence of transition metals, mainly nickel and iron, indicates corrosion problems. Traces of these ions are determined using Inline Preconcentration (MiPCT). After separation, post-column reaction with 4-(2-pyridylazo)resorcinol (PAR) allows VIS detection at 510 nm.

This e-book explains how Raman and near-infrared (NIR) spectroscopy enable rapid, nondestructive polymer analysis, ensuring high quality while reducing costs and waste.

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 coupling of ion chromatography and inductively coupled plasma mass spectrometry (ICP/MS) leads to a high-performance measurement system that masters several particularly challenging analyses. It enables for example reliable determination of element compositions, oxidation states and chemical bonds. This information is used, for example, for assessing the toxicity of medications, environmental and water samples as well as foods and beverages.

Propylene oxide (PO) is a major industrial product used in assorted industrial applications, mainly for the production of polyols (the building blocks for polyurethane plastics). Several production methods exist, with and without co-products. This white paper lays out opportunities to optimize PO production for safer and more efficient processes, higher quality products, and substantial time savings by using online process analysis instead of laboratory measurements.

«Dissolved oxygen» describes the amount of oxygen molecules (O2) which are dissolved in a liquid phase under certain conditions. In this white paper, two different methods for the analysis of dissolved oxygen, titration and direct measurement, are compared and contrasted to help analysts determine which method is more suitable for their specific applications. Here, we primarily focus on the determination of dissolved O2 in water. However, the same principle applies for other liquid phases such as non-alcoholic or alcoholic beverages.

Ion measurement can be conducted in several different ways, e.g., ion chromatography (IC), inductively coupled plasma optical emission spectrometry (ICP-OES), or atom absorption spectroscopy (AAS). Each of these are well-established, widely used methods in analytical laboratories. However, the initial costs are relatively high. In contrast, ion measurement by the use of an ion-selective electrode (ISE) is a promising alternative to these costly techniques. This White Paper explains the challenges which may be encountered when applying standard addition or direct measurement, and how to overcome them in order for analysts to gain more confidence with this type of analysis.

Ion chromatography mass spectrometry (IC-MS) is a powerful tool that can handle many challenging analytical tasks which cannot be performed adequately by IC alone. IC-MS is a robust, sensitive, and selective technique used for the determination of polar contaminants like inorganic anions, organic acids, haloacetic acids, oxyhalides, or alkali and alkaline earth metals. After separation of the sample components via IC, mass selective detection guarantees peak identity with low detection limits. The inclusion of automated Metrohm Inline Sample Preparation (MISP) allows not only water samples, but also chemicals, organic solvents, or post-explosion residues to be readily analyzed without need for extensive manual laboratory work. This White Paper explains the benefits of IC-MS over IC in certain cases, the hyphenation of IC and different MS systems, as well as related norms and standards.

This White Paper presents four different «green» sensors: the scTRACE Gold, screen-printed electrodes, the glassy carbon electrode, and the Bi drop electrode from Metrohm that can be used to determine low concentrations of heavy metals in different sample matrices, such as boiler feed water, drinking water, and sea water.