Application Finder

Determination of disinfection byproducts in water is a standard application for ion chromatography. Applying conductivity detection the separation of chlorite and bromate from chloride is crutial for μg/L detection limits. The combination of a Metrosep A Supp 7 - 250/4.0 and a Metrosep A Supp 16 Guard/4.0 lead to an improved separation. The Limit of Quantification for bromate is around 1 μg/L

Microbore columns with an inner diameter of 2 mm reduce the eluent consumption to about a quarter. Consequently, the detected peak areas of corresponding sample concentration are increased by a factor 4. In this report, the determination of anions in drinking water is described on a Metrosep A Supp 5 - 150/2.0 column.

Perchlorate is known as a potential contaminant in drinking water. Besides very few natural sources, it mainly originates from disinfectants, bleaching, propellants, etc. EPA method 314.0 requires to reach a method detection limit of 0.5 µg/L for perchlorate in reagent water. But also water with a very high content of total dissolved solids needs to be analysed by this method. Making use of the Metrosep A Supp 7 - 250/4.0 column fulfills all requirements of this method.

Cobalt is an essential element for humans because it is a component of vitamin B12. While small overdoses of cobalt compounds are only slightly toxic to humans, larger doses from 25–30 mg per day may lead to skin, lung, and stomach diseases, as well as liver, heart, and kidney damage, and even cancerous growths. The same is valid for nickel, which can lead to inflammation at higher concentrations. Drinking a large amount of water containing nickel can cause discomfort and nausea. In the EU the legislation specifies 0.02 mg/L as the limit value for the nickel concentration in drinking water. This concentration can be reliably determined with the method described in this Application Bulletin.

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.

EN ISO 10304-1 is one of the most important standards for the determination of the seven standard anions in water samples. Many other standards refer to EN ISO 10304-01 if anion determination by IC is required. This standard asks for a membrane filtration for samples to avoid bacteria and solids, if required. This application shows the determination of anions according EN ISO 10304-1 applying Inline Ultrafiltration. This setup avoids tedious manual sample filtration and handles any samples fully automatically.

Reducing the analysis time is a demanding task because it is accompanied by a parallel reduction of peak resolution. With a Microbore column 100 mm in length, standard cations in tap water can be determined in only 5 minutes. Strontium can also be determined by simply extending the run time to 6.5 min.

Excessive silica concentrations in the boiler feed water can lead to deposits on turbine blades and must therefore be avoided. Silica analysis is carried out via differential photometry using a leading-edge technology thermostatic cuvette module for non-sample contact at the detector. Typical concentration ranges for silica are 0–50 ppb and 0–1 ppm or higher.

Determination of bromide and phosphate in waste dump drainage water in the presence of very high concentrations of other ions and organic substances using anion chromatography with conductivity detection after chemical suppression and dialysis for sample preparation.

Boiler feed water is a working medium in thermal power plant. To keep corrosion low, the pH value should be in the slightly alkali range, which is why amines are added to the feed water. This addition must be monitored regularly. Also important is the monitoring of the sodium concentration, because an increase of this indicates that cooling water is seeping into the condenser. Ion chromatography with conductivity detection following sequential suppression is the optimum system for monitoring, particularly in combination with intelligent Sample Preconcentration and Matrix Elimination.

Boiler water analysis is an important task in power plant applications. Under the given conditions, the "Metrosep A Supp 10 - 100/4.0" column separates sulfite and sulfate without any organic modifier in the eluent. Even without any stabilizer, sulfite can be determined with a high reproducibility.

Determination of trace levels of lithium, sodium, ammonium, potassium, magnesium, and calcium in boiler feed water using cation chromatography with direct conductivity detection.

Water content determination by volumetric Karl Fischer titration is one of the most important analyses worldwide, particularly when it comes to food quality. This parameter has a major influence on the growth of microorganisms, and thus indirectly affects the storability of the raw materials and final products. Consistent quality is only possible with precise measurements during the process. This measurement is performed with the Metrohm Eco KF Titrator for flour, dough, and baked goods.

The water content of tablets determines the release of their active ingredients as well as their chemical, physical, microbial and shelf-life properties. Accordingly, the water content is of crucial importance and has to be accurately determined. This paper describes the straightforward determination of the water content using automated volumetric Karl Fischer titration (KFT). Tedious sample preparation steps are eliminated by using a high-frequency homogenizer that additionally serves as a stirrer. Prior to titration, the homogenizer comminutes the tablets directly in the KF solution. As the comminution process takes place directly in the hermetically sealed titration vessels, interference from atmospheric humidity does not occur. Even after 24 h in the vessels, the moisture content of four different tablet type samples was within 93…108% of the initially determined values. With a coefficient of determination of 0.99993 the KF method is highly linear for water amounts between 4 and 215 mg. For all investigated tablet types, KFT provides results that lie within the range expected by the manufacturer.

Determination of traces of fluoride, chloride, bromide, nitrate, and sulfate in a boiler feed water containing 10 mg/L ammonia using anion chromatography with conductivity detection after chemical suppression and inline sample preparation by cation exchange.

Determination of lithium, sodium, potassium, magnesium, and calcium in lake water using cation chromatography with direct conductivity detection.

Alkalinity is well-suited as a means of describing the capacity of a body of water to neutralize acid contaminations. It is therefore an important indicator for estimating the influence of contaminations on the ecological system.

The water content of ammonium and potassium peroxodisulphate is determined according to Karl Fischer using two-component reagents. To prevent unwanted side reactions the determinations are carried out at -20 °C. Because the potassium salt is insoluble in the solvent, a high-frequency homogenizer is used to disintegrate the salt particles.

Partial loop injection is a well known way of sample introduction to HPLC. In ion chromatography, it is not yet used to a large extent. Liquid handling with Metrohm's Dosino technology now enables to use partial loop injection on a highly reproducible and accurate level. It includes multi-level calibration out of one standard solution. This Application Note shows its use for parallel anion and cation determination in tap water applying one single Sample Processor. The anion results are shown in Application Note S–287.

Cation analysis in drinking water is a routine task in ion chromatography and can be achieved with a variety of separating columns. The use of a microbore Metrosep C 6 - 250/2.0 column with a high eluent concentration makes it possible to reduce analysis time to less than 12 minutes. Very symmetrical peaks with high sensitivity for the divalent cations are also achieved. Direct conductivity detection is applied.

Determination of sodium, potassium, calcium, and magnesium in the water soluble fraction of a washing powder using cation chromatography with direct conductivity detection.

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.

A setup that allows online sampling is crucial for immediate and contamination-free analysis of power plant water samples. This application recommends a setup that facilitates simultaneous anion/cation determinations. Automated inline sample preparation combines variable preconcentration (MiPCT) and calibration with a single multi-ion standard. AN-Q-004 displays the respective cation results.

This Application Note describes the automated determination of the water content in toothpaste using volumetric Karl Fischer titration (MATi 10).

The vaping and electronic cigarette industries are growing. The mixtures used in these products are usually called e-liquid, e-fluid, or e-juice. Toensure the quality of these e-liquids, testing the most important parameters is required. One important quality control parameter is water or moisture content.Water/moisture content determination by Karl Fischer titration (KFT) is an established and reliable procedure. Compared to other methods the advantages of KFT are its accuracy, speed, and selectivity. For high water content samples, such as e-liquids, volumetric KFT is the method of choice.In this Application Note a system for the fast and reliable determination of the water content in E-liquids is presented. This fully automated system performs the analysis including system preparation, blank, titer, and sample determination completely unattended. Hence, the workload of the operator is reduced to only weighing in the sample and placing the sealed sample vessels on the system.

The water content of methyl ethyl ketone peroxide is determined according to Karl Fischer using two-component reagents in order to prevent unwanted side reactions. (Separate solvent is used to ensure a high excess of sulphur dioxide and amine in the titration vessel.)

Neutralizing amines are added to adjust pH levels within the water-steam circuit of power plants to avoid corrosion-inducing conditions. This preventive maintenance can reduce costly and critical downtimes due to corrosion, however frequent monitoring of the amine chemistry is necessary to ensure conditions stay optimal. The 2060 IC Process Analyzer featuring the Metrohm intelligent Partial Loop Technique (MiPT) option is ideal for this application, with the ability to measure trace amounts of the analytes precisely and reliably through an automated method. The benefit of using IC is that multiple analytes can be monitored simultaneously, and here the ability to measure the presence of sodium next to the high ammonium or amine concentrations could indicate that cooling water is seeping into the circuit, indicating a problem upstream.

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

Maritime pore water contains sodium in the percentage range. The analysis of ammonia in this kind of sample requires a high column capacity and an exceptionally good separation of sodium and ammonia. These requirements are completely fulfilled by a 2 µL injection to the high-capacity Metrosep C 6 - 250/4.0 column.

Determination of NTA, EDTA, and DTPA in surface water and wastewater using ion pair chromatography with UV-detection after post-column reaction with the MSM.

Water activity is an important parameter to measure for non-sterile pharmaceutical quality and stability. The OMNIS NIR Analyzer provides this data within seconds.

This white paper demonstrates how OMNIS IC combines high analytical performance with advanced laboratory automation for drinking water analysis.

Partial loop injection is a well known way of sample introduction to HPLC. In ion chromatography it is not yet used to a large extent. Liquid handling with Metrohm's Dosino technology now enables to use partial loop injection on a highly reproducible and accurate level. It includes multi-level calibration out of one standard solution. This AN shows its use for parallel anion and cation determination in tap water applying one single Sample Processor. The cation results are shown in Applicatin Note C-133.

This Application Note describes the automated determination of the water content in liqueur (30% v/v) using volumetric Karl Fischer titration (MATi 10).

Drinking water analysis is strongly regulated by standards. In this Application Note, the cation determination according to ISO 14911 is shown. The Metrosep C 4 - 150/4.0 is the optimum separation column for this purpose.

This bulletin describes the determination of calcium, magnesium, and alkalinity in water by complexometric titration with EDTA as titrant. It is grouped into two parts, the potentiometric determination and the photometric determination.There are multiple definitions of the different types of water hardness. In this Application Bulletin, the following definitions are used: alkalinity, calcium hardness, magnesium hardness, total hardness, and permanent hardness. Explanations of these definitions and other expressions are provided in the Appendix.Determination of alkalinity during the photometric part is carried out in a separate acid-base titration before the complexometric titration of calcium and magnesium in water. Permanent hardness can be calculated from these values. The determination of calcium and magnesium in beverages (fruit and vegetable juices, wine) is also described.The photometric part includes the determinations of total and calcium hardness and thereby indirectly magnesium hardness using Eriochrome Black T and calconcarboxylic acid as indicators (in accordance with DIN 38406-3).

To determine water in crude oil, ASTM D4928 recommends coulometric Karl Fischer titration with the oven method, allowing full automation for high reproducibility.

The maximum contaminant concentrations (Maximal Contaminant Level, MCL) of inorganic arsenic and selenium species in drinking water should not exceed 10 and 50 µg/L, respectively. Given that each of the two elements occurs in two oxidation levels – trivalent and pentavalent – a separation step is necessary prior to ICP/MS detection. This Application Note shows the simultaneous determination of the two arsenic (arsenite and arsenate) and selenium species (selenite and selenate). Separation takes place on the Metrosep Dual 3 - 100/4.0 column.

Determination of bromide and bromate in drinking water using anion chromatography with MS detection.

Fast and handsome IC! Outstanding peak shapes on columns with the standard flow rate and a strong eluent. When the high-capacity Metrosep C 6 - 250/4.0 is used, this usually means long retention times. A strong eluent allows however the determination of the cations in drinking water in a short run time with very symmetrical peaks.

This Application Note shows how easy it is to determine water content in the pharmaceutical excipient lactose with reagent-free near-infrared spectroscopy.

In this application note, Karl Fischer titration is used to determine water content in sodium acetate trihydrate. The MATi 10 allows this determination to be automated, saving users time in the laboratory.

A setup that allows online sampling is crucial for immediate and contamination-free analysis of power plant water samples. This application recommends a setup that facilitates simultaneous anion/cation determinations. Automated inline sample preparation combines variable preconcentration (MiPCT) and calibration with a single multi-ion standard. AN-Q-005 shows the respective anion results.

Lithium-ion batteries must be completely free of water (concentration of H2O < 20 mg/kg), because water reacts with the conducting salt, e.g., LiPF6, to form hydrofluoric acid.The water content of several materials used in lithium ion batteries can be determined reliably and precisely by coulometric Karl-Fischer titration. In this Application Bulletin the determination for the following materials is described:raw materials for the manufacture of lithium-ion batteries (e.g., solvents for electrolytes, carbon black/graphite); electrode coating preparations (slurry) for anode and cathode coating; the coated anode and cathode foils as well as in separator foil and in the combined material; electrolytes for lithium-ion batteries;

Aluminum can be determined in drinking water by adsorptive stripping voltammetry at the HMDE using alizarin red S (DASA) as complexing agent. The method is linear up to 35 μg/L. The detection limit for this method is β(Al) = 1 μg/L, the limit of quantification is β(Al) = 3 μg/L. The sensitivity of the method cannot be increased by deposition.

The poster describes the water determination in pharmaceuticals using the Karl Fischer oven technique.

This Application Note shows how purity, degree of substitution and water content of carboxymethyl celluloses (CMC) can be determined conveniently and rapidly in a single measurement with Vis-NIR spectroscopy.

«High ionic water» is typically water containing a high concentration of chloride (e.g. seawater, brine), but this also describes water samples resulting from petrochemical processes. Due to the high chloride concentrations, the conductivity determination of minor ionic components is limited. Thus, minor anions like nitrite, bromide, and nitrate can elute under or on the tail of the large chloride peak, and their detection in low concentrations is hampered. However, combining conductivity and UV/VIS detection as described in ASTM D8234 enables the determination of anions that are UV active. Chloride does not interfere in this situation. The described technique enables the interference-free simultaneous determination of trace anions besides high chloride content.

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.

Determination of fluoride, chloride, nitrate, phosphate, and sulfate on a short column or the ions mentioned plus bromate and nitrite on a long column in water samples applying intelligent column-switching using anion chromatography with conductivity detection after sequential 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.

Determination of zinc, lithium, cobalt, sodium, ammonium, potassium, manganese, magnesium, and calcium in power plant feed water stabilized with 7 ppm monoethanolamine using cation chromatography with direct conductivity detection.

Near-infrared spectroscopy (NIRS) was used for quality control of skin creams. A model for the quantification of the water content was developed based on Karl Fischer titration (KF), enabling fast and reliable atline analysis and final product quality control.

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.

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).

Quantitation of the functionalization of a water-soluble polymer was achieved using a portable Raman spectrometer. The Raman spectrum provides strong, unique bands for both the initial and fully reacted polymer. This enables development of a simple, robust quantitative analysis of the percent polymer functionalization. This method is now routinely used in a manufacturing plant's quality control laboratory.

Hexavalent chromium (chromate) is known to be carcinogenic if inhaled, and suspected to be carcinogenic if ingested. EPA Method 218.7 allows to determine chromate in drinking water down to the sub-µg/L range (method detection limit, MDL = 15 ng/L). Post-column reaction with 1,5-diphenylcarbazide and subsequent visible detection at 530 nm is applied.

Water in steel-based cooling systems requires a pH value slightly above 7 to prevent corrosion. Often ammonium or organic amines are applied for pH adjustement. This application shows the separation of typical amines besides inorganic cations. Sample preconcentration applies combined Inline Preconcentration and Matrix Elimination (MiPCT-ME).

Swimming pool water needs to be thoroughly disinfected and this is often accomplished with ozonization. This process can generate harmful oxyhalides, the concentration of which must be monitored. Here the separation and determination of oxyhalides as well as standard anions are carried out using a column of the Metrosep A Supp 5 - 250/4.0 type. Quantification takes place using conductivity detection in accordance with sequential suppression.

This Application Note describes the determination of the water content in transformer oil using the oven technique.

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.

This Application Note describes the determination of the water content in gelatine using the oven technique.

Sorbic acid and benzoic acid and their salts are used as food preservatives (E200, E201, E201, E203 and E210, E211, E212, E213 respectively). The content of such preservatives in flavored bottled water may easily be analyzed by ion exclusion chromatography. This method determines the concentration of the respective acid and does not allow differentiating between the counter cations. The determination of sorbic acids and benzoic acid is achieved by conductivity detection after inverse suppression.

This poster describes the water determination in different biodiesel samples via direct coulometric titration, the Karl Fischer oven method and an automated KF pipetting system.

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.

Arsenic is ubiquitous in the earth’s crust in low concentrations. Elevated levels can be found in mineral deposits and ores. Arsenic from such deposits leaches into the groundwater in the form of arsenite (AsO33–) and arsenate (AsO43–), causing its contamination. As(III) is more toxic than As(V) and shows higher mobility in the environment. The selective determination of this species is possible using the method described in this document.With a limit of detection (LOD) of 0.3 μg/L, anodic stripping voltammetry allows speciation, i.e. the specific determination of As(III). While atomic absorption spectroscopy (AAS) (and competing methods) can only determine the total element concentration, anodic stripping voltammetry is selective to the As(III) oxidation state. The determination is carried out on the scTRACE Gold electrode.

Lead is known to be highly toxic, and lead salts are easily resorbed by humans. Cases of chronic lead poisoning caused by lead metal used in the water piping system are well known. Therefore, the control of drinking water for lead content is of utmost importance. The Lead and Copper Rule (LCR) published by the USEPA (United States Environmental Protection Agency) states an action limit of 15 μg/L lead for drinking water. Using a portable voltammetric instrument, lead can be determined in these concentrations directly at the point of sampling.

With the advent of electric automobiles, the demand for lithium batteries and with it the demand for lithium material will increase sharply. Brine lakes and hard silicate minerals are numbered among the most important sources of lithium. This Application Note addresses cation determination in seepage water from lithium minerals. Alkali and earth alkali metals are separated in the lithium digestions on the Metrosep C Supp 1 - 250/4.0 column, with subsequent conductivity detection after sequential suppression.

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 EN ISO 18127.

Only coulometric Karl Fischer titration can determine low water contents with sufficient accuracy.This Application Bulletin describes the direct determination according to ASTM D6304, ASTM E1064, ASTM D1533, ASTM D3401, ASTM D4928, EN IEC 60814, EN ISO 12937, ISO 10337, DIN 51777, and GB/T 11146. The oven technique is described according to ASTM D6304, EN IEC 60814, and DIN 51777.

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.

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

The human daily intake of boron from food and beverages is approximately 2 mg. This is far below any toxic level. Some plants, however, are extremely sensitive to boron concentrations above 1 mg/L, e.g., strawberries, blackberries. As seawater contains 4 to 5.5 mg/L of boron, desalination is required to remove surplus boron besides other ions. This application shows the determination of boron (as borate) by ion-exclusion chromatography with conductivity detection after inverse suppression. The method has been optimized to get a sufficient fluoride/borate separation.

In this application note, a fully automated system is presented which allows the determination of several parameters according to various standards within one analysis. These include conductivity (ISO 7888, EN 27888, ASTM D1125, EPA 120.1), the pH value (EN ISO 10523, ASTM D1293, EPA 150.1), alkalinity (EN ISO 9963, ASTM D1067, EPA 310.1), and Ca/Mg content (ISO 6059, ASTM D1126, EPA 130.2). Additionally, the system transfers the required sample volume into an external titration vessel for the analysis, reducing manual sample preparation. Furthermore, all sensors can be automatically calibrated and the titer of each titrant can also be determined.

Seawater analysis with conductivity detection is difficult due to the high excess of chloride. Especially analyzing for nitrite and bromide, UV/VIS detection is preferred as chloride is not interfering with nitrite at 218 nm. This AN shows the determination of all three UV-absorbing anions in an artificial seawater.

In this application note, a fully automated system is presented which allows the determination of several parameters according to various standards within one analysis. These include conductivity (ISO 7888, EN 27888, ASTM D1125, EPA 120.1), pH value (EN ISO 10523, ASTM D1293, EPA 150.1), alkalinity (EN ISO 9963, ASTM D1067, EPA 310.1), and chloride content (ISO 9297, ASTM D512, EPA 325.3). Additionally the system transfers the required volume of sample into an external titration vessel, further reducing manual sample preparation. Furthermore, all sensors can be calibrated automatically and the titer of each titrant can also be determined.

In this application note, a fully automated system is presented which allows the determination of several parameters according to various standards within one analysis. These include conductivity (ISO 7888, EN 27888, ASTM D1125, EPA 120.1), pH value (EN ISO 10523, ASTM D1293, EPA 150.1), alkalinity (EN ISO 9963, ASTM D1067, EPA 310.1), Ca/Mg (ISO 6059, ASTM D1126, EPA 130.2), and chloride (ISO 9297, ASTM D512, EPA 325.3). Additionally the system transfers the required volume of sample into external titration vessels for the different analyses, reducing manual sample preparation. Furthermore, all sensors can be automatically calibrated and the titer of each titrant can also be determined.

Fresh coconut water quality is influenced by crop location, harvest timing, and storage duration, creating challenges for consistent industrial production. This application describes the analysis of the parameters Brix, conductivity, turbidity, pH value, and salinity in coconut water with the OMNIS NIR Analyzer Liquid. Near-infrared spectroscopy (NIRS) enables rapid, reagent-free multiparameter analysis without sample preparation, reducing reliance on conventional laboratory testing.

Malachite green (MG) is a textile dye with effective fungicidal properties, however it is acutely toxic and its metabolites persist in the flesh of fish and mammals, making it a threat to the human food chain. The EU has concluded that contaminated foods containing levels higher than 2 μg/g MG constitute a credible health risk, and several countries have banned malachite green as an aquaculture additive. Despite tight regulation, seafood products contaminated with MG continue to find their way to consumers.Using Misa (Metrohm Instant SERS Analyzer) to ensure food safety, the rapid and highly sensitive detection of malachite green is achieved in a facile assay format.

Nitrite can be determined polarographically after its conversion to diphenylnitrosamine (C6H5)2NNO. Potassium thiocyanate is used as a catalyst in order for the conversion to proceed rapidly and quantitatively. The reaction takes place in acid solution at a pH value of approx. 1.5. The limit of quantification is 5 μg/L NO2-.

Ion chromatography with PCR and UV/VIS detection provides a highly specific and sensitive method for bromate analysis, meeting EPA Method 317 and ISO 11206 requirements.

Determination of chloride, nitrite, bromide, nitrate, and sulfate in water for infusion solution production using anion chromatography with conductivity detection after chemical suppression.

Vinylene carbonate is a widely used lithium-ion battery electrolyte additive that requires strict moisture control to maintain battery performance and lifetime. Accurate moisture quantification was historically limited by side reactions, complicating the analysis. The introduction of alcohol-free coulometric Karl Fischer reagents now enables precise, reproducible moisture determination, facilitating more reliable control of additive and electrolyte quality during manufacturing.

A safer way to monitor moisture content in crude distillation unit overhead fractions is with inline near-infrared spectroscopy using the 2060 The NIR-Ex Analyzer.

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

Determination of Na2O and SiO2 in water glass by potentiometric titration with HCl using the Sb electrode.

Accurate determination of Fe(II) and Fe(III) in water is crucial for many industries. Cathodic sweeping voltammetry (CSV) offers a robust, cost-effective solution.

Compounds with carbonyl groups can be prone to oxidation for which reason their stability often decreases during storage or processing. The method presented here is suitable for the determination of aldehydes and ketones sparingly soluble in water.Samples are dissolved in deionized water. After a reaction with the hydroxylamine hydrochloride at 50 °C, carbonyl groups are quickly and accurately determined by potentiometric titration using the dUnitrode and sodium hydroxide as titrant.

With Hydranal™ NEXTGEN FA reagents, the water content in ketones can be determined quickly and reliably. Compared to other existing KF reagents for ketones on the market, the side reactions are measurably better suppressed.

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.

Cd, Pb, and Cu can be determined in one run in acetate buffer by anodic stripping voltammetry (ASV).

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 low levels of chloride (to approximately 5 mg/L Cl-) by thermometric titration.

Determination of fluoride, chloride, nitrite, nitrate, and sulfate in an effluent sample using anion chromatography with direct conductometric detetction.

Determination of sodium dodecylsulfate (SDS, sodium laurylsulfate) using anion chromatography with direct conductivity detection.

Cr(III) forms an electrochemically active complex with diethylenetriaminepentaacetic acid (DTPA), so does Cr(VI) after in situ reduction on the surface of the HMDE. Depending on the sample preparation procedure and the waiting time after the addition of the complexing agent, the different chromium species can be differentiated:Total active chromium [total concentration of Cr(VI) and free Cr(III)]:The measurement is carried out immediately after the addition of DTPA.; Cr(VI): Between the addition of DTPA and the start of the analysis a minimum waiting time of 30 min is necessary. During this waiting time the Cr(III)-DTPA complex becomes electrochemically inactive.; Cr(III): The difference between the total active Cr and Cr(VI).; Totalchromium: Determination of total active Cr after UV digestion.;

VoltIC Professional 1 is the perfect combination of voltammetry and ion chromatography for the fully automated, simultaneous analysis of anions, cations, and heavy metals (e.g., Zn, Cd, Pb, Cu). The multiple-parameter analysis uses the same "Liquid Handling" elements and a shared sample changer, thus saving on space and costs.

Sulfate is precipitated by reaction with an acidified barium chromate solution. The excess barium chromate is precipitated by basification with ammonia solution. Residual soluble chromate equivalent to the sulfate content of the sample is titrated with a solution of standard ferrous ion to a thermometrically determined endpoint.

High-Performance Liquid Chromatography (HPLC) and Ion Chromatography (IC) are commonly used in the pharma, food, and environmental sectors to analyze samples for specific components and to verify compliance with norms and standards. However, users of HPLC may run into the limitations of this technique, e.g., when analyzing standard anions or certain pharmaceutical impurities. This white paper outlines how such challenges can be overcome with IC.

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.

This poster looks at the possibility to modify the existing EPA Method to meet California's rigorous public health goal (PHG) of 0.02 µg/L. After optimizing instrument settings and method parameters, a method detection limit (MDL) of 0.01 µg/L is obtained.

A combination of the 850 Professional IC and the 872 Extension Module Liquid Handling opens the field of Metrohm’s online monitoring by IC. In this application, Inline Preconcentration is coupled to Matrix Elimination (MiPCT-ME). By removing excess matrix components, corrosive anions can be sensitively determined. Additionally, this technique allows automated calibration using a single multi-ion standard solution. Online trace analysis for chloride and sulfate is possible for several different sample lines.

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.

The Se(IV) concentration can be determined by cathodic Stripping Voltammetry (CSV) in an ammonium sulfate electrolyte. The analysis also functions in the presence of Cu. Se(IV) is determined in the first step. In order to register the entire content of Se, Se(VI) species are first reduced to Se(IV). This is handled by the 909 UV Digester at a pH value of between 7 and 9. The method requires practically no reagents and permits selenium speciation.

Cadmium, lead, and copper can be determined simultaneously in oxalate buffer by anodic stripping voltammetry (ASV) after digestion with sulfuric acid and hydrogen peroxide. Tin present in the sample does not interfere with the determination of lead.For the voltammetric determination of tin please refer to Application Bulletin no. 176.

In modern days, a new breed of energetic (explosive) materials is emerging. Traditional aromatic nitrates are still in use, but there is dire need of analytical techniques for energetic materials in the chemical class of peroxides, azo etc. This presentation will demonstrate the use of a modern HPLC system with traditional detector (DAD) and also coupled with mass spectrometry for the analysis of abovementioned various classes of energetic materials.

The Eco IC is an entry-level instrument that is particularly suitable for routine operations and water analysis. It is equipped with a conductivity detector and can be used both with and without chemical suppression. This Application Note describes the determination of anion content with the Metrosep A Supp 17 - 250/4.0 column. This column model is particularly suitable for water analysis at room temperature.

Chromium is extracted from chromite ore and is an important part in the production of stainless steel. Chromium is mainly divalent, trivalent and hexavalent in its compounds. In contrast to chromium(III), which is an important trace element and one that is only sparingly soluble in water, hexavalent chromium is extremely toxic and very water-soluble. Cr(VI) is furthermore an important raw material for industry. It must be determined rapidly and precisely in the lower µg/L range in wastewater. Metrohm Applikon offers an array of process analyzers for the analysis of wastewater streams which determine chromium precisely and reproducibly using photometry.

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.

Methylamine (MMA), dimethylamine (DMA), and trimethylamine (TMA) in methylpyrrolidone using Metrohm Inline Matrix Elimination.

Coagulation and flocculation are an essential part of treating both drinking water and wastewater. Aluminum salts such as aluminum sulfate and polyaluminum chloride (PAC) are often used for this purpose. For the precise application and exact dosage of the flocculant, it is important to accurately determine its aluminum content. In this Application Note, the aluminum content is accurately and reliably analyzed based on ABNT NBR 11176 using the 859 Titrotherm equipped with a Thermoprobe HF and sodium fluoride as titrant.

This Application Bulletin describes methods for the polarographic and voltammetric determination of small quantities of chromium in water, effluent water and biological samples. Methods for the sample preparation for various matrices are given.

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.

This White Paper gives an overview of the energy-intensive nitrification process that converts ammonia into less harmful nitrogen compounds at wastewater treatment plants (WWTPs). It displays the results from a field test at a WWTP, showcasing the positive influence of single-method process analyzers on the efficiency of the nitrification process.

The new DIN draft standard 38407-53 outlines TFA analysis in water using direct injection LC-MS/MS, enabling quantification from 0.1–3.0 μg/L as shown in this Application Note.

Using disposable 11COND screen printed electrodes and electrochemical impedance spectroscopy, conductivity in drinking water can be measured using only 100 µL samples.

This Process Application Note deals with online measurements of ammonia, nitrite, and nitrate in wastewater treatment plants. These nitrogen compounds are analyzed simultaneously using a drift-free colorimetric measurement in a multi-parameter process analyzer from Metrohm Process Analytics.

The stability of the Metrosep A Supp 5 - 250/4.0 column was determined in long-term laboratory tests. Two injection series each were run on six days in a row. Each series was comprised of nine tap water injections, three check standard injections and six tap water injections. The IC system was shut down on the seventh day of each series. As a whole, the IC system ran over 10 weeks and counted a total of 2,150 injections. The results show an outstanding reproducibility and verify the high column stability.

The column stability of the microbore version of the Metrosep A Supp 5 - 250/2.0 was determined in long-term laboratory tests. Two injection series each were run on six days in a row. Each series was comprised of nine tap water injections, three check standard injections and six tap water injections. The IC system was shut down on the seventh day of each series. As a whole, the IC system ran over 12 weeks and counted a total of 2,650 injections. The results show an outstanding reproducibility and verify the high column stability.

The method describes the determination of Cr traces in a range between 1 ... 250 μg/L. The method is based on the adsorption of a Cr(lll)-diphenylcarbazonate complex on the Ultra Trace graphite rotating disk electrode (RDE). Organic compounds present in samples (e.g. natural waters) have a strong interfering effect. So they have to be removed by e.g. UV digestion. The determination is made by adsorptive stripping voltammetry in the DC (direct current) measuring mode. Purging with nitrogen is not necessary. The determinations work well also in high salt concentration solutions.

This Application Bulletin describes the determination of titanium by adsorptive stripping voltammetry (AdSV) using mandelic acid as complexing agent. The method is suitable for the analysis of ground, drinking, sea, surface and cooling waters, in which the concentration of titanium is of importance. The methods can, of course, also be used for the trace analysis in other matrices.The limit of detection is approx. 0.5 µg/L.

Determination of fluoride, glycolate, acetate, formate, chloride, nitrite, nitrate, and sulfate in the primary cycle water of a pressurized water reactor (PWR) using anion chromatography with conductivity detection after chemical suppression calibrated with Metrohm Inline Calibration.

This Application Note presents DPV as a sensitive, selective method for detecting heavy metals in water, detailing setup, parameters, and advantages over other techniques.

This Application Bulletin describes the methods for the determination of uranium by adsorptive stripping voltammetry (AdSV) according to DIN 38406 part 17. The method is suitable for the analysis of ground, drinking, sea, surface and cooling waters, in which the concentration of uranium is of importance. The methods can, of course, also be used for the trace analysis in other matrices.Uranium is determined as chloranilic acid complex. The limit of detection in samples with low chloride concentration is about 50 ng/L and in seawater about 1 µg/L. Matrices with high chloride content can only be analyzed after reduction of the chloride concentration by means of a sulfate-loaded ion exchanger.

This Application Bulletin describes the voltammetric determination of the elements iron, copper and vanadium. Fe as well as Cu and V can be determined as catechol complex at the HMDE by adsorptive stripping voltammetry (AdSV). Fe(II) and Fe(III) are determined as Fe(total) with the same sensitivity for both species in either phosphate buffer or PIPES electrolyte. Cu and V can be determined in PIPES buffer.The methods are primarily suitable for the investigation of ground, drinking and surface waters, in which the concentration of these metals is important. But the methods can naturally also be used for trace analysis in other matrices.The limit of detection for all three elements in PIPES buffer is 0.5 ... 1 µg/L, for iron in phosphate buffer it is approx. 5 µg/L.

Determination of formate, acetate, propionate, isobutyrate, butyrate, isovalerate, valerate, and capronate added to tap water using anion chromatography with conductivity detection after suppression. The MCS is placed upstream of the chemical suppressor to remove interfering CO2.

The method described allows the determination of W(VI) traces in the range 0.2 to 50 µg/L (ppb). Traces of organic compounds present in the samples (e.g. natural waters) interfere. They have to be removed by UV digestion (e.g. 705 UV Digester). Interference by Fe(III) up to a concentration of 100 mg/L is eliminated by reduction to Fe(lI) with ascorbic acid. If the amount of Cu(II) in the sample exceeds the amount of W(VI) by a factor of 200 or more, the Cu ions have to be bound with thiourea. Moreover, the concentration of Cu(II) should not exceed 5 mg/L. The determination is made by adsorptive stripping analysis in the DP mode.

Sulfide and sulfite can be determined polarographically without any problems. For sulfide, polarography is performed in an alkaline solution, for sulfite in a slightly acidic primary solution. The method is suitable for the analysis of pharmaceuticals (infusion solutions), wastewater/flue gas water, photographic solutions, etc.

Although the known photometric methods for the determination of ammonia/ammonium are accurate, they require a considerable amount of time (Nessler method 30 min, indophenol method 90 min reaction time). A further disadvantage of these methods is that only clear solutions can be measured. Opaque solutions must first be clarified by time-consuming procedures. These problems do not exist with the ion-selective ammonia electrode. Measurements can be easily performed in waste water, liquid fertilizer, and urine as well as in soil extracts. Especially for fresh water and waste water samples several standards, such as ISO 6778, EPA 350.2, EPA 305.3 and ASTM D1426, describe the analysis of ammonium by ion measurement. In this Application Bulletin, the determination according to these standards is described besides the determination of other samples as well as some general tips and tricks on how to handle the ammonia ion selective electrode. Determination of ammonia in ammonium salts, of the nitric acid content in nitrates, and of the nitrogen content of organic compounds with the ion-selective ammonia electrode is based on the principle that the ammonium ion is released as ammonia gas upon addition of excess caustic soda:NH4+ + OH- = NH3 + H2OThe outer membrane of the electrode allows the ammonia to diffuse through. The change in the pH value of the inner electrolyte solution is monitored by a combined glass electrode. If the substance to be measured is not present in the form of an ammonium salt, it must first be converted into one. Organic nitrogen compounds, especially amino compounds are digested according to Kjeldahl by heating with concentrated sulfuric acid. The carbon is oxidized to carbon dioxide in the process while the organic nitrogen is transformed quantitatively into ammonium sulfate.

Chromate (Cr(VI)) or hexavalent chromium is carcinogenic. Its use is restricted. Chromate has to be analyzed in a large range of products starting with drinking water, wastewater (e.g., from leather production), over toys to RoHS-regulated substances. Besides ion chromatographic determination applying conductivity detection, the method described here is suitable especially for lower concentrations.

The automated system MATi 13 determines the permanganate index in all kind of water samples according to EN ISO 8467. The high degree of automation (e.g., automated sample addition, automated titer and blank value determination) minimizes errors and guarantees robust and reproducible results.

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).

Increased fluoride concentrations in water may cause tooth damage, growth disorders, and bone deformation. According to the World Health Organization (WHO), concentrations above 1.5 mg/L are critical.One possible source of fluoride is landfills. Rain washes out harmful substances from landfills which can enter the groundwater. The leachate from landfills should thus be monitored for the fluoride concentration.Ion measurement is a fast and inexpensive method to determine the fluoride content in water samples compared to other methods such as ion chromatography. This Application Note describes a reproducible and accurate measurement of the fluoride content using the fluoride ion-selective electrode with an OMNIS system.

This Application Bulletin describes two methods for the determination of iron at the Multi Mode Electrode.Method 1, the polarographic determination at the DME, is recommended for concentrations of β(Fe) > 200 μg/L. For this method the linear range is up to β(Fe) = 800 μg/L.For concentrations < 200 μg/LMethod 2, the voltammetric determination at the HMDE, is to be preferred. The detection limit for this method is β(Fe) = 2 μg/L, the limit of quantification is β(Fe) = 6 μg/L. The sensitivity of the method cannot be increased by deposition.Iron(II) and iron(III) have the same sensitivity for both methods.These methods have been elaborated for the determination of iron in water samples. For water samples with high calcium and magnesium concentrations such as, for example, seawater, a slightly modified electrolyte is used in order to prevent precipitation of the corresponding metal hydroxides. The methods can also be used for samples with organic loading (wastewater, beverages, biological fluids, pharmaceutical or crude oil products) after appropriate digestion.

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

Kjeldahl nitrogen is a typical titration application that follows digestion and ammonia distillation. The ASTM Standard D8001 now offers an alternative applying persulfate digestion followed by IC determination. No distillation is required. In addition, the method enables the determination of total nitrogen and total phosphorus. We show the results of control samples containing organic substances. As these substances are dissolved in ultrapure water, the nitrogen concentration found corresponds to Total Nitrogen and Kjeldahl Nitrogen.

Determination of bromate in water using anion chromatography with UV/VIS detection after post-column reaction (PCR) with o-dianisidine reagent (described in EPA 317.0).

This poster describes a method for automated and precise dosing of liquid samples into the Karl Fischer titration cell using Metrohm Dosino liquid handling technology. First, the titer was automatically determined with ultrapure water. The same dosing procedure proved valuable for the automated water determination in highly viscous water-glycol fluids and low-boiling organic solvents such as n-pentane. Lastly, the method copes with the labor-intensive and human error-prone suitability test stipulated in chapter 2.5.12 in the European Pharmacopoeia.

Corrosion in the water-steam circuit of power plants leads to shorter lifetimes of most metal components and potentially dangerous situations. Flow Accelerated Corrosion (FAC) is a specific case, leading to thinned pipes and elevated Fe concentrations in the circuit. Additionally, metal transport issues such as with Cu from copper heat exchangers can lead to deposition on the high pressure turbine blades, decreasing their efficiency. Current methods can monitor but not prevent these issues, and analysis times are extremely long (up to three weeks). In combination with the power plant’s Distributed Control System (DCS), online monitoring of Fe and Cu with the 2060 Process Analyzer from Metrohm Process Analytics ensures that corrosion can be controlled before it affects the power plant efficiency, ultimately decreasing downtime and lowering maintenance costs. Results are offered within 20 minutes, allowing fast adjustments to the water-steam circuit to protect company assets.

Caprolactam is an important polymer used for the production of Nylon 6, which is the base material for industrial fibers. Due to its commercial significance, many different synthesis methods have been developed over the years. Caprolactam is hygroscopic and water soluble, therefore it is important to have a reliable analysis technique for water determination. Analyzing the water content by conventional methods requires each sample to be weighed, dissolved, heated, and titrated. Compared to the primary method, near-infrared spectroscopy (NIRS) offers unique advantages: it generates reliable results within seconds, but it does not need any sample preparation nor does it create chemical waste.

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 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 traces of zinc and iron(II) in the presence of lithium, sodium, ammonium, potassium, calcium, and magnesium in boiler water using cation chromatography with direct conductivity detection.

This Application Bulletin describes a voltammetric method for the determination of aluminum in water samples, dialysis solutions, sodium chloride solutions and digestion solutions (e.g. of lyophilisates). The method utilizes the complexation of the Al3+ ion by Calcon (Eriochrome blue black R). The formed complex can easily be reduced electrochemically at 60 °C. The limit of quantitation depends on the purity of the reagents used and is approx. 5 µg/L.

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

Determination of total phosphate in wastewater after digestion with peroxodisulfate using anion chromatography with conductivity detection after chemical suppression.

Determination of thiooctanoate in wastewater using anion chromatography with conductivity detection after chemical suppression.

The determination of anions in tap water is a simple IC application. Here it is used to present Metrohm's intelligent Pick-up Technique (MiPuT). MiPuT enables the injection of volumes of minimum size from very small sample quantities. In the present case, two volumes of 10 µL from a sample 100 µL in size are used for anion and cation analysis, respectively. The calibration takes place through the injection of various volumes of a single standard solution. AN-C-141 describes the corresponding cation determination.

Determination of sulfate in wastewater after nitric acid combustion using anion chromatography with conductivity detection after chemical suppression.

Determination of iodide in wastewater (dye industry) using anion chromatography with amperometric detection at the silver electrode and dialysis for sample preparation.

Determination of nitrite and nitrate in wastewater using anion chromatography with conductivity detection after chemical suppression.

Total chromium can be determined in wastewater samples. UV digestion is necessary to remove interfering organic matter before the analysis. Complete oxidation of Cr(III) to Cr(VI) is guaranteed by an additional UV irradiation step at pH > 4.

Tin can be determined in wastewater by anodic stripping voltammetry (ASV) in oxalate buffer after addition of methylene blue. Samples with organic substances have to undergo UV digestion before analysis. Samples with higher concentrations of metals can be diluted before digestion.

The concentration of Fe(total) is determined in wastewater after UV digestion. The method is suitable for iron concentrations down to the low μg/L range. Stripping voltammetry is not applicable for this method. Fe(II) and Fe(III) generate signals with identical sensitivity.

MATi 11 (MATi = Metrohm Automated Titration) is a completely configured system for water content determination in solid or liquid samples using automated volumetric Karl Fischer titration. It contains a Polytron PT 1300 D for the homogenization of the samples. Up to 53 samples are analyzed directly in 120 mL titration beakers. The samples are weighed in the titration beaker and sealed with aluminum foil and a foil holder so that they neither lose nor absorb water.

This Application Bulletin describes the method of near-infrared spectroscopy in diffuse reflection for the purpose of determining residual moisture in a lyophilized pharmaceutical product. Numerous sample vials containing freeze-dried pharmaceuticals were spiked with varying amounts of water for calibration purposes. The resulting differences in the absorption wavelengths of the OH-oscillation were correlated with the water content determined by Karl Fischer titration using the algorithm of multiple linear regression (MLR).

Hexavalent chromium (Cr(VI)) is regarded as being toxic and potentially carcinogenic. Its concentration in drinking water should therefore be kept as low as possible. The determination of Cr(VI) is performed using ion chromatography. The separation takes place on the Metrosep A Supp 10 - 250/2.0 separation column. The presence of Cr(VI) is determined photometrically following post-column reaction (PCR) with diphenylcarbazide.

Test measurements on water standards are performed with an OMNIS KF Titrator and Karl Fischer reagents Aquagent® Complet 5 and Methanol Fast from Scharlau.

Ion chromatographic determination of sulfide in wastewater is performed using amperometric detection and an alkali eluent to ensure the stability of the sulfide. Measurements are performed in single-potential or direct current (DC) amperometric mode. It is the best-known and most sensitive amperometric measuring method and also provides, in addition to a high selectivity, a large selection of working electrodes.Sulfide determination is performed on a Metrosep A Supp 10 - 100/4.0 type column; a silver electrode is used as the working electrode.

Nickel and cobalt can be determined in seawater by adsorptive stripping voltammetry (AdSV) at the HMDE.

Determination of nickel and cobalt in wastewater samples through adsorptive Stripping Voltammetry (AdSV). The wastewater samples first undergo a UV digestion in accordance with DIN 38406 Part 16.

In power plants, corrosion is the primary factor leading to costly and critical downtimes. In a nuclear power plant, a separate water circuit known as the Pressurized Water Reactor (PWR) ensures radioactive material stays contained while still transferring heat and energy to the other circuits. Boric acid and lithium hydroxide are added specially to the PWR circuit in amounts which can complicate other analytical measurements. Lithium prevents corrosion and must be monitored, along with other cations such as zinc, nickel, and ammonium. In order to measure these cations online at sub-µg/L range in a single analysis, the 2060 IC Process Analyzer is offered with combined Inline Preconcentration and Inline Matrix Elimination. Several cations can be analyzed in a single injection, with automated sample preparation making precise and reliable measurements easier.

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.

Determination of borate in seawater using ion-exclusion chromatography with suppressed conductivity detection after inline matrix elimination.

Selenium is determined by cathodic stripping voltammetry (CSV) at the hanging mercury drop electrode (HMDE). Se(IV) is deposited on the surface of the mercury drop in sulfuric acid electrolyte under addition of copper ions as Cu xSe y.Wastewater samples containing organic contaminants have to be digested by UV irradiation before analysis. In addition, the sample has to undergo a second irradiation step at pH 7−9 to reduce Se(VI) to Se(IV), since only Se(IV) is electrochemically active.

Determination of calcium and magnesium in seawater. The method is suitable for determining the effect of caustic soda and alumina refinery aluminate solutions on the calcium and magnesium content of seawater.

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

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

Determination of nitrite, nitrate, and phosphate in seawater from a shrimp farm using anion chromatography with conductivity detection after chemical suppression and subsequent UV/VIS detection.

Determination of water in automotive lubricating oils.

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;

The determination of cations in tap water is a simple IC application. Here it is used to present Metrohm's intelligent Pick-up Technique (MiPuT). MiPuT enables the injection of volumes of minimum size from very small sample quantities. In the present case, two volumes of 10 µL from a sample 100 µL in size are used for anion and cation analysis, respectively. The calibration takes place through the injection of various volumes of a single standard solution. AN-S-302 describes the corresponding anion determination.

Determination of sulfide in wastewater by direct potentiometry with the Ag/S ion-selective electrode.

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.

Determination of bromide, nitrate, and phosphate in wastewater using anion chromatography with conductivity detection after chemical suppression and dialysis for sample preparation.

Cd and Pb can be determined in seawater samples in the ng/L concentration range by anodic stripping voltammetry on a mercury film electrode (MFE).

Mercury can be determined in wastewater by anodic stripping voltammetry (ASV) on a gold rotating disk electrode (Au RDE). After the addition of hydrochloric acid and hydrogen peroxide, digestion is done by UV irradiation.

Thallium in wastewater is determined in acetate buffer in presence of EDTA by anodic stripping voltammetry (ASV). Samples with organic substances have to undergo UV digestion before analysis.

The concentration of Cu in seawater is determined by anodic stripping voltammetry (ASV) in acetate buffer on a mercury film electrode (MFE). Gallium is added to overcome zinc interferences.

This Application contains information regarding titer determination in Karl Fischer titration, in particular regarding the water standard suitable for a titer determination and for the correct handling of the same.Titer determination for Karl Fischer titrants is indispensable, because the titer is subject to changes caused by the humidity in the air. The frequency of the determination depends on the titrant and the tightness of the system.The titer has the unit mg/mL in Karl Fischer titration. The value calculated in a titer determination indicates how many milligrams of water react on one milliliter of titrant.

This Application Bulletin describes the stripping analysis of Ag at the rotating disk electrode (RDE) with glassy carbon tip (GC) or Ultra Trace graphite tip. In routine operation, the determination limit lies at approx. 10 μg/L Ag, with careful work 5 μg/L Ag can be obtained. After appropriate digestion, silver determination is also possible with samples containing a relatively high proportion of organic substances (e.g. wine, foodstuffs etc.). The method has been developed primarily for water samples (well, ground and wastewater, desilvering solutions of the photographic industry).

Determination of chloride, bromide, and sulfate in synthetic seawater using anion chromatography with conductivity detection after chemical suppression.

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

Ion chromatography trace analysis of anions in seawater is difficult, due to the high chloride concentrations. In contrast to chloride, nitrite, bromide and nitrate absorb UV radiation in the low wavelength range, thus enabling a UV detection of these three anions. This Application Note describes the separation on a column of the Metrosep Carb 2 - 100/4.0 type with a sodium chloride eluent. This minimizes the influence of the surplus chloride and enables low detection limits.

Determination of water in moist particulate solids such as cobalt oxyhydroxide.

Determination of nitrite, nitrate, sulfite, and sulfate in wastewater containing high levels of chloride using anion chromatography with conductivity detection after chemical suppression and after inline chloride removal.

This Application Bulletin provides information regarding the MATi 10 (Metrohm Automated Titration) system. MATi 10 is a completely configured system for automatic volumetric Karl Fischer titration with which the water content in liquid and solid samples can be determined. Up to 24 samples can be analyzed directly in 75 mL titration vessels. The samples are weighed into the titration vessels and covered with an aluminum foil. This prevents falsification of the water content.

Determination of sodium, ammonium, methylamine, guanidine (Gu), and aminoguanidine (Agu) in wastewater using cation chromatography with direct conductivity detection.

Zinc, cadmium, lead, and copper can be determined in wastewater samples after UV digestion by anodic stripping voltammetry (ASV) according to DIN 38406 part 16.

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

MATi 4 (Metrohm Automated Titration) is a configured system for automated water content determination in liquid samples using coulometric Karl Fischer titration. The maximum sample volume is 5 mL. Up to 160 samples are filled in glass vials and sealed with lids. This ensures that the water content in the samples remains constant. The samples are aspirated and transferred into the coulometric cell through a needle. The tiamo™ software controls the system.

Sulfide and cyanide are toxic anions. Their trace determination in any kind of water samples, especially in wastewater, is requied for safety reasons. However, metal traces present in the eluent can mask target anions due to complexation. The addition of a stronger complexing agent to the eluent mask these metal cations enabling interference free determaination. This application is mainly used for the analysis of cyanide and/or sulfide in water. However, it also fulfills the requirements of ASTM D2036 for the determination of total, amenable, weak acid dissociable cyanides. The determination of cyanide and sulfide require an alkaline eluent and amperometric detection. This Application Note describes a new column/eluent combination for optimized separation. The combination consists of the Metrosep A Supp 10 - 100/4.0 column and a sodium hydroxide eluent containing a trace of EDTA for transition metal complexation. This yields in better peak shape and detection limits below 0.1 μg/L.

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

Incineration flue gas requires treatment such as wet scrubbing. The 2060 VA Process Analyzer monitors heavy metals in the scrubbing water, ensuring compliance.

Determination of sulfide in mining wastewater using anion chromatography with UV detection.

Determination of fluoride, chloride, nitrate, sulfite, phosphate, and sulfate in wastewater 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.

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.