Applikationer

The determination of the physical and chemical parameters as electrical conductivity, pH value, p and m value (alkalinity), chloride content, the calcium and magnesium hardness, the total hardness, as well as fluoride content are necessary for evaluating the water quality. This bulletin describes how to determine the above mentioned parameters in a single analytical run.Further important parameters in water analysis are the permanganate index (PMI) and the chemical oxygen deman (COD). Therefore, this Bulletin additionally describes the fully automated determination of the PMI according to EN ISO 8467 as well as the determination of the COD according to DIN 38409-44.

Maleic and fumaric acid can be reduced electrochemically to succinic acid. In acidic solutions a differentiation of the two acids is not possible since both are reduced at the same potential. On the other hand, separation at pH 7.8...8.0 is easily possible since fumaric acid is now more difficult to reduce at the lower proton concentration (as a result of cis-trans isomerism) than maleic acid.

The formol number represents a further parameter for the characterization of fruit and vegetable juices. As this is merely an index (the formalin number does not deal with the molecular size, nor with the quantity of amino acids), the conditions of the titration can be adapted to meet practical needs. This concerns mainly the pH value of the endpoint of the SET titration (pH = 8.5, pH = 9.0, pH = 9.2, etc.).

Mixtures of aluminum and magnesium ions can be analyzed automatically using potentiometric titration. The excess DCTA is back-titrated with copper(II) sulfate solution after the addition of 1,2-diaminocyclohexanetetraacetic acid (DCTA) and complex formation. The ion-selective copper electrode is used here as the indicator electrode. First, the aluminum is determined in acidic solution and then the magnesium in alkali solution.

This Bulletin describes the voltammetric determination of aluminum in water samples down to a concentration of 1 μg/L. An aluminum complex is formed with alizarin red S (DASA) and enriched at the HMDE. The following determination employs differential pulse adsorptive stripping voltammetry (DP-AdSV). Disturbing Zn ions are eliminated by addition of CaEDTA.

This Bulletin, using practical examples, indicates how the user can achieve optimum pH measurements. As this Bulletin is intended for actual practice, the fundamentals - which can be found in numerous books and publications - are treated only briefly.

4-Carboxybenzaldehyde, in the following referred to as 4-CBA, can be reduced directly at the dropping mercury electrode (DME) in an ammoniacal solution. After a very simple sample preparation it is now possible to determine the concentration of 4-CBA in terephthalic acid quickly and precisely by polarography down to the lower ppm range.

After the degradation of biological samples (e.g. milk, wool, etc.), it is often important to know the cystine/cysteine ratio. This Application Bulletin describes the simultaneous, polarographic determination of the two amino acids. The determination is performed in perchloric acid solution at the DME. Samples with a high protein content require that the determination is performed in an alkaline solution.

Thiourea forms highly insoluble compounds with mercury. The resulting anodic waves are used for the polarographic determination of thiourea. For the analysis of very small quantities (µg/L), cathodic stripping voltammetry (CSV) is used. Differential Pulse measuring mode is used in both cases.

This Bulletin describes the simultaneous potentiometric titration of free boric acid and free tetrafluoroboric acid in nickel plating baths. After addition of mannitol, the formed mannitol complexes are titrated with sodium hydroxide solution. The determination is carried out directly in the plating bath sample; nickel and other metal ions do not interfere.

Formaldehyde can be determined reductively at the DME. Depending on the sample composition it may be possible to determine the formaldehyde directly in the sample. If interferences occur then sample preparation may be necessary, e.g. absorption, extraction, or distillation.Two methods are described. In the first method formaldehyde is reduced directly in alkaline solution. Higher concentrations of alkaline or alkaline earth metals interfere. In such cases the second method can be applied. Formaldehyde is derivatized with hydrazine forming the hydrazone, which can be measured polarographically in acidic solution.

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.

Polyurethanes are one of the most commonly used types of plastic. They are produced by the reaction of raw polyols with isocyanates. Depending on the starting material a wide variety of plastics can be obtained. The determination of the acid value, hydroxyl value, and isocyanate content plays an important part in the analysis of raw materials for plastics.The acid number of polyol raw material is usually used in quality control to ensure batch-to-batch uniformity. Additionally it is used as correction factor for calculating the true hydroxyl number. In this Application Bulletin the determination of the acid number according to ASTM D4662 and ASTM D7253 is described.One raw material for polyurethanes are polyols. Polyols contain multiple hydroxyl groups. Therefore, hydroxyl number of a raw material directly correlates to the amount of polyols present and it is thus an important quality control parameter. In this Application Bulletin the determination of the hydroxyl number according to ASTM E1899 and DIN 53240-3 is described.As polyols react stoichiometrically with isocyanates, the knowledge of the isocyanate content is an important quality parameter for the production of polyurethanes. In this document the determination according to EN ISO 14896 method A, ASTM D5155 method A and ASTM D2572 is described.

This document outlines Rancimat testing for both liquid and solid food samples, including direct and PEG methods, for oxidation stability QC in the food industry.

This Application Bulletin describes the determination of the thermostability of PVC in accordance with ISO 182 Part 3 using the dehydrochlorination method with the 895 Professional PVC Thermomat. The instrument permits fully automatic determination of the stability time. The test is suitable for monitoring the manufacture and processing of PVC products manufactured in the injection molding process, for their final clearance, characterization and for the comparison of PVC products and for testing the effectiveness of heat stabilizers.

This Bulletin provides an overview of the potentiometric titer determination of current titrants. Many publications only describe methods with color indicators. However, the titration conditions chosen for the titer determination should resemble those used for the actual analysis as closely as possible. The tables contain suitable titrimetric standard substances and electrodes for selected titrants as well as additional information. Following this, an example is given to show what an SOP for a titer determination could look like.

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).

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.

The sample preparation for ion chromatography is divided into steps which should generally be implemented to preserve the column and into steps which should be performed to obtain an improved chromatogram. The goal is to have the test substance in ionic form in solution without the presence of interfering substances.

This Application Bulletins describes the determination of nicotinamide (vitamin PP), a vitamin of the B series. Instructions for the determination in solutions (e.g. fruit juice), vitamin capsules and multivitamin tablets are given. The linearity range of the determination is also specified. The limit of detection is approximately 50 μg/L nicotinamide.

This Application Bulletin describes the polarographic determination of folic acid, a vitamin of the B series, also known as vitamin B9 or vitamin BC. Instructions for the determination in solutions (e.g. fruit juice), vitamin capsules and multivitamin tablets are given. The linear range of the determination is also specified. The limit of detection is approx. 75 µg/L folic acid.

This Application Bulletins describes the polarographic determination of thiamine (vitamin B1). The procedure allows an analysis in monovitamin preparations. The linear range of the determination is also given. The limit of detection is approx. 50 µg/L thiamine.

This Application Bulletin describes the polarographic determination of riboflavin (vitamin B2). The procedure allows an analysis in monovitamin preparations. The limit of determination is approx. 100 μg/L.

This Application Bulletin describes …

This Bulletin gives a survey of standard methods from the field of water analysis. You will also find the analytical instruments required for the respective determinations and references to the corresponding Metrohm Application Bulletins and Application Notes. The following parameters are dealt with: electrical conductivity, pH value, fluoride, ammonium and Kjeldahl nitrogen, anions and cations by means of ion chromatography, heavy metals by means of voltammetry, chemical oxygen demand (COD), water hardness, free chlorine as well as a few other water constituents.

This Bulletin describes the fully automated determination of uranium according to the method of Davies and Gray: Uranium(VI) is reduced in concentrated phosphoric acid solution with iron(II) to form Uranium(IV). With molybdenum as a catalyst, the excess iron(II) is oxidized with nitric acid. The nitrous acid that is formed is destroyed with sulfamic acid before uranium(IV) is titrated with a potassium dichromate solution in the presence of a vanadium catalyst.

This Application Bulletins describes the polarographic determination of pyridoxine (vitamin B6). The method given allows determination in monovitamin and in some multivitamin preparations. The linear range of the analysis is also specified. The limit of detection is approx. 100 µg/L pyridoxine · HCI.

The Bulletin describes the determination of the following parameters in wine: pH value, total titratable acid, free sulfurous acid, total sulfurous acid as well as ascorbic acid (vitamin C) and other reductones.

This Bulletin describes the determination of arsenic by anodic stripping voltammetry (ASV) at the rotating gold electrode. A determination limit of 0.5 μg/L can be achieved with 10 mL sample solution. A differentiation between the As(III) concentration and the total arsenic concentration can be made by appropriate selection of the deposition potential. The analyses are performed with a special gold electrode whose active surface is located laterally; c(HCl) = 5 mol/L is used as supporting electrolyte. For the determination of the total arsenic content, As(III) and As(V) are reduced at -1200 mV by nascent hydrogen to As0, which is preconcentrated on the electrode surface. If the deposition is carried out at -200 mV then only As(III) is reduced; this allows the differentiation between total arsenic and As(III). During the subsequent voltammetric determination the preconcentrated As0 is again oxidized to As(III).

The titrimetric determination of nonionic surfactants on the basis of polyoxyethylene adducts (POE adducts) is described in the Bulletin. The basis for the determination is the transfer of the nonionic surfactant into a pseudo-cation compound and its precipitation titration with sodium tetraphenylborate (Na-TPB). The NIO electrode is used for the indication of the potentiometric titration. This Bulletin describes determinations in raw products, formulations and wastewater and draws attention to special features, possibilities, limits and disruptions.

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).

The effectiveness of antioxidants can be expressed as antioxidant activity. It can be readily determined using the Rancimat method. This is accomplished by first determining the induction time of a mixture made up of hog fat and the antioxidant to be investigated and then by determining the corresponding time for hog fat alone. The quotient expresses the efficiency of the respective antioxidant and is referred to as the antioxidant activity index (AAI).This Application describes the determination of the antioxidant activity index of five common antioxidants.

Anionic surfactants can be titrated with cationic surfactants and vice-versa. The Bulletin describes a multitude of substances that can be determined in this fashion and specifies the respective working conditions and parameters. In contrast to the classic two-phase titration in accordance with Epton, the titration with the anionic and cationic surfactants electrodes can be performed without chloroform. Furthermore, the equivalence point of the titration is difficult to determine in some cases with the Epton method and the titration cannot be automated.In many cases, a surfactant ISE is a remedy that is both environmentally friendly and suitable here. It was developed specially for application with potentiometrically indicated surfactant determinations.

This Bulletin describes a simple method for the determination of the calcium content in dairy products. The use of CuEGTA and the ion-selective copper electrode (Cu ISE) as indicator electrode allows the determination to be performed without time-consuming sample preparation. If the complexing agent EDTA is used as titrant instead of EGTA, the sum of calcium and magnesium is obtained. The magnesium content can then be calculated from the difference between the results of the two titrations.

Determination of the oxidation stability of foods with a low fat content is a challenge. As an alternative, the oxidation stability can be specified indirectly. To accomplish this, a determination is made as to the extent that a sample that has been mixed with a fat as a standard solution, e.g., hog fat, will change the oxidation stability of that standard solution. This is accomplished by first determining the induction time of the mixture made up of hog fat and the sample and then by determining the corresponding time for the lard alone. The quotient is referred to as the stability index (SI).

This Application Bulletin describes the determination of cadmium and lead at a mercury film electrode (MFE) by anodic stripping voltammetry (ASV). The mercury film is plated ex situ on a glassy carbon electrode and can be used for up to one day. With a deposition time of 30 s, the limit of detection is ß(Cd2+) = 0.02 µg/L and ß(Pb2+) = 0.05 µg/L. The linear working range for both elements goes up to approx. 50 μg/L using the same deposition time.

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.

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.

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.

Diazepam belongs to the 1,4-benzodiazepine group of compounds, which are used for medical purposes as tranquilizers and antidepressants. This Bulletin describes the determination of diazepam in tablets and body fluids (blood, serum, urine) by means of differential pulse polarography. If a Britton-Robinson buffer pH = 2.8 with a methanol volume fraction of 20% is used as the supporting electrolyte then a pronounced reduction peak is obtained at -0.73 V; this allows diazepam concentrations even below 0.05 µg/mL to be determined in blood. The necessary sample preparation steps are also dealt with in this Bulletin.

Cinchocaine (dibucaine) is used in the form of ointments or injection solutions as a local anaesthetic. Its base is soluble in diethyl ether; its hydrochloride, on the other hand, is insoluble in diethyl ether but easily soluble in water. This Bulletin describes the determination of cinchocaine in ointments, creams and injection solutions by means of differential pulse polarography. An acetate buffer pH = 4.8 is used as the supporting electrolyte. The limit of quantitation and the linear working range of the method are given. The necessary sample preparation steps are also dealt with in this Bulletin.

This Application Bulletin describes the determination of zinc at a mercury film electrode (MFE). Zinc can also be determined simultaneously with cadmium and lead. The determination of copper at the MFE is not possible. The mercury film is plated ex-situ on a glassy carbon electrode and can be used for half a day up to one day.Zinc can be determined at the mercury film electrode by anodic stripping voltammetry (ASV). The presence of copper, which is naturally present in many samples, affects the determination of zinc due to the formation of an intermetallic compound. As a result the determined concentrations of zinc are too low. The addition of gallium can eliminate the interference to a certain extent since the intermetallic complex of gallium and copper is more stable than the complex of zinc and copper.With a deposition time of 10 s, the limit of detection is β(Zn2+) = 0.15 μg/L. The linear working range goes up to approx. 300 μg/L.With the deposition time of 10 s the method is suitable for samples between 10 μg/L and 150 μg/L Zn content. For samples with lower concentrations the results are more reliable if the deposition time is increased to e.g. 30 s. Samples with higher concentrations have to be diluted.

The two potentiometric titration methods described here allow the determination of the content of commercial betaine solutions. Neither method is suitable for determining the betaine content of formulations. The possibilities and limits of both methods are described and distinctive features and possible sources of interference are mentioned. The Bulletin explains the most important theoretical principles and is intended to help users to develop their own product-specific titration methods.

This Bulletin describes the determination by ion chromatography of anions, particularly fluoride, chloride, nitrite, bromide, nitrate, and sulfate using the Hamilton PRPX100 IC anion column without chemical suppression.

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.

The present Bulletin offers an overview of the multitude of surfactants and pharmaceuticals that can be determined with potentiometric titration. Metrohm provides five different surfactant electrodes for indicating the titration endpoint: the Ionic Surfactant, the High Sense, the Surfactrode Resistant, the Surfactrode Refill and the NIO Surfactant electrode. The manufacture of the respective titrants and their titer determination are described in detail. In addition to this, the Bulletin contains a tabular overview of more than 170 proven applications from the area of surfactant and pharmaceutical analysis. This guideline leads you reliably to your destination: At a glance you can see from the table which surfactant electrode and which titrant are optimally suitable for your product.

On the basis of a multitude of practical examples, this Bulletin describes the potentiometric two-phase titration of ionic surfactants in raw materials and many other formulations.Two surfactant electrodes – the Surfactrode Resistant and the Surfactrode Refill – make it possible to perform this type of surfactant titration, analogous to the classic "Epton titration", with a high degree of automation. The achieved results correlate very well with those of Epton titration. The toxic, carcinogenic and environmentally hazardous chloroform can be replaced by other solvents such as methyl iosbutyl ketone or n-hexane.

Two-phase titration with potentiometric indication is a universal method for the determination of ionic surfactants in detergents. The results obtained are comparable to those with the classic two-phase titration in accordance with Epton (mixed indicator system disulfine blue / dimidium bromide). The present Bulletin addresses various parameters that could have an influence on potentiometric surfactant titration. The information provided makes it possible for the user to determine precisely the anionic surfactant content in practically all formulations.

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.

In an acidic solution (containing NH4F * HF, Al(NO3)3 / KNO3) sodium forms NaK2AlF6 which precipitates in an exothermic solution, enabling analysis by thermometric titration. Several foods were analyzed, namely bouillon, gravy, tomato ketchup, corn chips, pretzel sticks as well as crackers. The reproducibility of the results was good. After weighing in and adding solutions, samples were crushed with a polytron to ensure homogeneity in the measuring solution. Relative standard deviations were between 0.08% and 3.75%. In addition to this application bulletin, you can find more information on thermometric sodium determination in foods in our application video available on YouTube:https://youtu.be/lnCp9jBxoEs

The presented Application Bulletin describes the apparatus and methods that are used for acid-base analysis of whole blood and blood plasma by Joergensen and Stirum. Evaluation of the measured data is performed with a software sold by Komstar AG.

This Application Bulletin describes methods for checking the condition of electrodes for surfactant titration. For testing electrodes used for ionic surfactant titration (Ionic Surfactant electrodes), sodium dodecyl sulfate (SDS) is determined using TEGO®trant. Conversely, for testing electrodes used for cationic surfactant titration (Cationic Surfactant electrodes), TEGO®trant is titrated with SDS.For non-ionic surfactant electrodes (NIO surfactant electrode), PEG 1000 is titrated with sodium tetraphenylborate (STPB).For testing Surfactrode Resistant and Surfactrode Refill electrodes, titrations of SDS with TEGO®trant are performed. Suitable criteria for the test are the height of the potential jump and the shape of the titration curve.Key word: NaPh4B

Sulfate can be rapidly and easily titrated thermometrically using a standard solution of Ba2+ as titrant. In industry, the widespread procedure is applied to the determination of sulfate in wet-process phosphoric acid. This bulletin deals with the determination of sulfate in granular fertilizers such as MAP (monoammonium phosphate), DAP (diammonium phosphate) and TSP (triple superphosphate). Results are reported as percentage of elemental sulfur, %S.

Sulfate can be rapidly and easily titrated thermometrically using a standard solution of Ba2+ as titrant. In industry, the widespread procedure is applied to the determination of sulfate in wet-process phosphoric acid.

The determination of the total causticizer, sodium carbonate and aluminum oxide contents in (Bayer) process liquors can be accomplished with high precision and speed by using the 859 Titrotherm in a thermometric acid-base titration. A complete titration takes approximately 5 minutes.The procedure is an automated adaptation of the traditional Watts-Utley method, and is similar to the VanDalen-Ward thermometric titration method, but with the added advantage that the analysis can also be performed for the carbonate content of the liquor.

Phosphate can be rapidly and easily titrated thermometrically using a standard solution of Mg2+ as titrant. The phosphate-containing solution is basified and buffered with NH3/NH4Cl solution before titration. The formation of insoluble MgNH4PO4 is exothermic. The method is a titrimetric adaptation of a classical gravimetric procedure. This bulletin deals with the determination of phosphate in phosphoric acid and granular fertilizers such as MAP (monoammonium phosphate), DAP (diammonium phosphate) and TSP (triple superphosphate). Results are reported as percentage of P and P2O5.

In titration, the titrant reacts with the analyte either exothermically (gives off heat) or endothermically (absorbs heat). The Thermoprobe measures the temperature change during titration. When all of the analyte has reacted with the titrant, the temperature of the solution will change, and the endpoint of the titration is indicated by an inflection in the temperature curve. Catalytically enhanced titrations using paraformaldehyde as catalyst are based on the endothermic hydrolysis of the paraformaldehyde in the presence of excess hydroxide ions. Edible oils are dissolved in a mixture of toluene and 2-propanol (1:1) and titrated with standardized TBAH (0.01 mol/L) in 2-propanol to a catalytically enhanced endpoint.

The phosphoric acid content can be easily titrated with a standardized solution of 2 mol/L NaOH. The interfering calcium content in phosphoric fertilizer can be eliminated by adding a saturated oxalate solution.

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.

The presented titration system can be used for the fully automated determination of the hydroxyl number (HN) according to ASTM E1899 and EN ISO 4629-2. The method allows, the determination of polyols and oxooils without boiling under reflux or other sample preparation and is therefore a big benefit for laboratories that have to cope with a high sample throughput.The standards EN 15168 and DIN 53240-3 relay on the same analysis method as in ASTM E1899.

This bulletin describes a procedure to determine the bromine index (BI) using coulometric titration. The bromine index is the fraction of reactive unsaturated compounds (mostly C=C double bonds) in hydrocarbons encountered in the petrochemical industry. The double bonds are split with the attachment addition of bromine.

This bulletin deals with the automated determination of calcium and magnesium in commercially available finished milk products using a 859 Titrotherm and a 814 USB Sample Processor. Calcium and magnesium in milk can be rapidly and easily titrated thermometrically using a standard solution of Na4EDTA as titrant.Thermometric titrations are conducted under conditions of constant titrant addition rate. The molarity of the titrant is computed automatically in tiamo (software) using the SLO command. Results are reported as mg Ca and Mg/100 mL.

This bulletin discusses automated determination of sodium in milk products available to the public using a 859 Titrotherm and a 814 USB Sample Processor. The sodium content of milk can be rapidly and easily titrated thermometrically with a standard solution of Al3+ as titrant. Thermometric titrations are conducted under conditions of constant titrant addition rate. The molarity of the titrant is computed automatically in tiamoTM (software) with the SLO command. Results are reported as mg Na/100 mL. In addition to this application bulletin, you can find more information on thermometric sodium determination in foods in our application video available on YouTube:https://youtu.be/lnCp9jBxoEs

This bulletin deals with the automated determination of mixtures of HNO3, HF and H2SiF6 in the range of approximately 200-600 g/L HNO3, 50-160 g/L HF, and 0-185 g/L H2SiF6 using thermometric titration.Etch acid mixtures containing HNO3, HF and H2SiF6 from the etching of silicon substrates can be analyzed in a sequence of two determinations using the 859 Titrotherm. The first determination involves a direct titration with standard c(NaOH) = 2 mol/L, followed by a back titration with c(HCl) = 2 mol/L. This determination yields the H2SiF6 content plus a value for the combined (HNO3+HF) contents. The second determination consists of a titration with c(Al3+) = 0.5 mol/L to determine the HF content. For freshly made up mixtures of HNO3 and HF containing no H2SiF6, a linked two-titration sequence is employed. Results from the two determinations are used by tiamoTM to yield individual results for HNO3, HF and H2SiF6.

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).

The determination of the acid number plays a significant role in the analysis of petroleum products. This is manifested in the numerous standard procedures in use over the world (internal specifications of multinational companies, national and international specifications of ASTM, DIN, IP, ISO, etc.). These procedures differ mainly in the composition of the used solvents and titrants.This bulletin describes the determination of the acid number in petroleum products by applying different types of titration.The potentiometric determination is described according to ASTM D664, the photometric according to ASTM D974 and the thermometric titration according to ASTM D8045.

This Application Bulletin shows the determination of the total base number in petroleum products by applying different titration types according to various standards.

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.

The Rancimat method determines the oxidation stability (OSI) and antioxidant capacity (SI) of solid foods. OSI measurements are performed directly, with extracted isolated fat, or via the polyethylene glycol method. SI can be determined when the sample is mixed with a reference of antioxidant-free fat.

The present Application Bulletin contains NIR applications and feasibility studies for NIRSystems devices in the chemical industry. Qualitative and quantitative analyses of a wide variety of samples are part of this bulletin. Each application describes the instrument that was originally used for the analysis, as well as the system recommended for the analysis and the results that were achieved thereby.

The present Application Bulletin contains NIR applications and feasibility studies using NIRSystems devices in the pharmaceutical industry. Qualitative and quantitative analyses of a wide variety of samples are part of this bulletin. Each application describes the instrument that was originally used for the analysis, as well as the system recommended for the analysis and the results that were achieved thereby.

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

The present Application Bulletin contains NIR applications for the determination of important parameters for pulp and paper quality analysis. Each application describes the instrument that was originally used for the analysis, as well as the system recommended for the analysis and the results that were achieved thereby.

The present Application Bulletin describes applications that use near-infrared spectroscopy. Each application describes the used and alternatively deployable spectrometer as well as analysis conditions and results and, where available, information on feasibility studies.

The present Application Bulletin elucidates several applications for the polymer industry that can be carried out with the aid of NIR instruments. This Bulletin contains analyses of a wide range of parameters in a very large array of samples. The hydroxyl number is one of the best-known of the parameters that can be determined rapidly using near-infrared spectroscopy. The determination of the hydroxyl number in different areas and in different polyol types is also a part of this Bulletin. Each application describes the sample and the instrument that was originally used for the analysis, as well as the recommended instruments and the results.

This Application Bulletin describes the determination of arsenic in water samples by anodic stripping voltammetry using the scTRACE Gold sensor. This method makes it possible to distinguish between As(total) and As(III). With a deposition time of 60 s, the limit of detection for As(total) is 0.9 µg/L, for As(III) it is 0.3 µg/L.

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.

The Application Bulletin describes the determination of suppressor in acid copper baths by smartDT. The determination of suppressor with dilution titration (DT) involves numerous additions with standard solution or sample to reach the evaluation ratio. Usually fixed, equidistant addition volumes are used. With smartDT, variable addition volumes are used that are dynamically calculated by the software. At the beginning, the volumes are bigger. Towards the evaluation ratio, the addition volume becomes smaller to guarantee a good accuracy of the result. The operator defines the first and the smallest addition volume to be used. All volumes in between are calculated by the software considering the progress of the determination. The time saving with smartDT compared to a classic DT with fixed addition volumes can be up to 40%. smartDT is suitable for nonlinear regression and quadratic regression as well as linear interpolation. It can be used for determination of suppressor in acid copper baths as well as in tin and tin-lead baths and works with 1, 2, and 3 mm Pt working electrodes. A 800 Dosino is required for the automatic addition of suppressor standard or sample. The method can also be used in fully automated systems.

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.

This Application Bulletin describes the determination of inorganic mercury in water samples by anodic stripping voltammetry using the scTRACE Gold sensor. With a deposition time of 90 s, calibration is linear up to a concentration of 30 µg/L; the limit of detection lies at 0.5 µg/L.

This Application Bulletin compares the unique focusing technology of the portable Metrohm Raman system "Mira" with conventional methods. The method described here is called Orbital Raster Scan (ORS). Experiments show the advantages of ORS technology, using determination and quantification of medicines as an example. It improves the reproducibility of the Raman signals from targeted, active, pharmaceutical ingredients (APIs) in effervescent, cold medicines. Shorter analysis times and an improved, consistent assignment of spectra of the known medicine with the help of a spectral library are further advantages of ORS technology.

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 determination of the total acid number in various oil samples by catalytic thermometric titration as per ASTM D8045.

This Bulletin describes the automatic measurement of conductivity in water samples with low electrical conductivity in accordance with USP<645>. Conductivity measurement is demonstrated on the example of ultrapure water, which is used, among other things, to produce injection solutions in the pharmaceutical sector.

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.

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.

This Application Bulletin describes the determination of Sn(II) in presence of Sn(IV) by anodic stripping voltammetry (ASV). Using an electrolyte containing fluoride, Sn(IV) gives no signal, so that a speciation is possible. The limit of detection is 2.5 µg/L.

Lead is known to be highly toxic and lead salts are easily absorbed by creatures. By interfering with enzyme reactions,lead can affect all parts of the human body. It can cause severe damage to brain and kidneys and can cross the bloodbrain barrier. 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. In many countries (e.g., EU, USA), the limit for lead in drinking water is between 10 and 15 μg/L. These concentrations can reliably be determined with the method described in this Application Bulletin. The determination is carried out by anodic stripping voltammetry at a silver film applied to the scTRACE Gold electrode.

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;

Heavy metals, particularly cadmium and lead, are known to be highly toxic to humans. Therefore, controlling the cadmium and lead content in drinking water is of utmost importance. In many countries, the limit in drinking water for cadmium is between 3–5 µg/L, and for lead it is between 5–15 µg/L. These trace concentrations can reliably be determined with the method described in this Application Bulletin. The determination is carried out by anodic stripping voltammetry (ASV) using the non-toxic Bi drop electrode in a slightly acidic electrolyte.

Iron is an essential element in the human diet and is found in many natural and treated waters. Therefore, the World Health Organization (WHO) does not issue a health-based guideline value for iron. Higher concentrations of iron in surface waters can indicate the presence of industrial effluents or outflow from other operations and sources of pollution. Because of this, precise, rapid, and accurate iron determination at low concentrations in environmental and industrial samples is of great importance. This can be achieved with the method described in this Application Bulletin.

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.

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

This method is applicable to all samples containing glycerin in the absence of other triols or other compounds that react with periodate to produce acidic products. Glycerin may be determined in the presence of glycols. A periodate solution reacts slowly with diols and triols in acidic aqueous media at room temperature. A quantitative amount of formic acid is generated from the reaction with glycerin (a triol). The reaction with diols produces neutral aldehydes. The amount of formic acid generated by this reaction is determined by titration against sodium hydroxide.

Automatic sample handling and analysis is very convenient for routine measurements on large number of samples. Metrohm offers a wide range of high performance liquid handling devices that can be combined with the Autolab product range and can be directly controlled by the NOVA software.

The Metrohm 800 Dosino is the workhorse of any automated liquid handling setup. This instrument can be conveniently used in combination with the NOVA software and integrated conveniently with electrochemical measurements performed with the Autolab systems.

The Metrohm 858 Professional Sample Processor is a robotic liquid handling system capable of handling large series of samples automatically. This instrument provides a platform that can be directly controlled by the NOVA software and combined with the Autolab potentiostat/galvanostat for automated high-throughput electrochemical measurements.

A nickel metal hydride battery, abbreviated NiMH, is a type of rechargeable battery similar to a nickel-cadmium (NiCd) battery but, for the anode, instead of cadmium, it has a hydrogen absorbing alloy. Like in NiCd batteries, nickel is the cathode. The voltage output of such packs is directly proportional to the number of single cells in the pack. In some cases, the total voltage can exceed the maximum of 10 V that is measurable by the Autolab potentiostat/galvanostat. To apply and measure voltages greater than 10 V, we have developed a voltage multiplier that increases the voltage range of the Autolab.

Lithium-ion (Li-ion) batteries are one of the most important energy storage devices in the market. A typical Li-ion battery is usually composed of one or more cells. Characterization of Li-ion cells and batteries usually involves the galvanostatic charge and discharge during various cycles.

This Application Note outlines GITT, a key technique for studying Li-ion battery kinetics, OCV, and diffusion, using INTELLO for streamlined control and analysis.

During charge and discharge of a Li-ion battery, lithium ions are transported from one electrode through the electrolyte to the other electrode. Knowing the chemical diffusion coefficient of electrode materials is crucial. The potentiostatic intermittent titration technique (PITT) is one of the most used techniques to retrieve insights on the diffusion coefficient of the electrode active materials.

The main components of a battery are the positive and negative electrodes, together with the electrolyte, which provides only the ionic conductivity. The most common electrolytes are in the liquid state. Therefore, a separator is needed to provide a physical separation between the electrodes. The separator is soaked with electrolyte. The MacMullin number is a parameter used to determine the quality of a separator, in terms of ionic conductivity, when soaked with an electrolyte. The MacMullin number can be calculated, using the results of data fitting of two EIS experiments and the geometric factors of the measurement cells. In this application note, a commercial electrolyte is employed, together with a porous filter, used as a separator.

The TSC SW closed and TSC battery cells are compact systems designed for measurement of air or moisture sensitive materials, such as those materials used in rechargeable batteries. These cells offer well-controlled environment for the in-temperature measurement of solid and gel like materials in contact with metal electrodes in planar geometry. For example, battery active materials, ionically conductive solid-state electrolytes and battery separators can be tested using these cells. In this experiment, standard resistors of 100 Ω are used in both cells to understand the cell effects, if any, on the measurements.

The DuoCoin Cell Holder is introduced. EIS measurements on a commercial coin cell battery are performed. Differences in impedance between the four-terminal configuration and two-terminal configuration is highlighted, putting in evidence the importance of having a direct four-terminal configuration, when low-impedance DUTs are investigated.

In this application note, we demonstrate how to determine the binary diffusion coefficient of a commercial liquid binary lithium ion battery electrolyte based on a galvanostatic pulse polarization method.

This application note presents the experimental details and an overview of the most important findings from the EIS and CV experiment to study the structure of a model solid electrolyte interface forming on a planar glassy carbon electrode in contact with a typical organic battery electrolyte.

In this application note, we demonstrate how to determine the through-plane tortuosity τ of a commercial lithium ion battery cathode material with known porosity and coating thickness, based on the electrochemical impedance spectroscopy (EIS) method.

In this application note, we demonstrate how to determine the lithium ion transference number of a commercial liquid binary lithium ion battery electrolyte, based on the very-low-frequency electrochemical impedance spectroscopy (VLF-EIS) method.

In battery research, electrochemical impedance spectroscopy (EIS) is a necessary tool to investigate the processes occurring at the electrodes. With a common three-electrode battery, EIS can be performed sequentially first at one electrode and then at the other electrode.

This Application Note explains how researchers can determine the underlying chemistry and potential failure mechanisms from cycle testing batteries with INTELLO.

This Application Note discusses differential capacity analysis (DCA) and its impact on enhancing battery performance, with a focus on using the INTELLO platform.

This application shows how EIS, combined with INTELLO and NOVA, tracks changes in internal battery resistance across SOC levels to study performance and aging mechanisms.

Determination of 3-dimethylamino-1-propylamine in cocoamidopropyl betaine using cation chromatography with direct conductometric detection.

Determination of sodium, potassium, calcium, and magnesium in a drip feeding formula using cation chromatography with direct conductivity detection and dialysis as sample preparation.

Determination of sodium, potassium, calcium, and magnesium in instant baby milk powder using cation chromatography with direct conductivity detection and dialysis for sample preparation.

Determination of calcium and magnesium in high-purity sodium chloride using cation chromatography with direct conductivity detection.

The use of an appropriate full scale together with the zero function of the 732 IC Detector minimizes baseline noise dramatically. Much lower detection limits are achieved.

Determination of sodium, ammonium, potassium, calcium, and magnesium in 4% boric acid using cation chromatography with direct conductivity detection.

Determination of calcium and magnesium in rock extracts using cation chromatography with direct conductivity detection.

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.

Determination of aluminum using cation chromatography, post-column reaction and UV detection.

Determination of lead, zinc, indium, cadmium, cobalt, ammonium, potassium, manganese, magnesium, and calcium using cation chromatography with direct conductivity detection.

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

Determination of sodium, ammonium, and potassium in polyethers using cation chromatography with direct conductivity detection.

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

Determination of zinc, sodium, ammonium, and manganese in the presence of magnesium and calcium in an extract of a zinc compound using cation chromatography with direct conductivity detection.

Determination of sodium, potassium, iron(II), magnesium, and calcium in an extract of monoethylene glycol using cation chromatography with direct conductivity detection.

Determination of nickel, zinc, cobalt, iron(II), and manganese in lithium bromide using cation chromatography with UV/VIS detection (520 nm) after post-column reaction with PAR.

Determination of sodium, ammonium, potassium, calcium, and magnesium in betaine using cation chromatography with direct conductivity detection.

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 sodium, ammonium, potassium, calcium, and magnesium in a grapefruit soft drink using cation chromatography with direct conductivity detection after advanced dialysis for inline sample preparation.

Determination of sodium, ammonium, potassium, calcium, and magnesium in a functional fruit juice using cation chromatography with direct conductivity detection after advanced dialysis for inline sample preparation.

Determination of zinc, sodium, calcium, and magnesium in an industrial bath containing cooling lubricants using cation chromatography with direct conductivity detection.

Determination of sodium, potassium, calcium, magnesium, putrescine, cadaverine, and histamine in a wine sample using cation chromatography with direct conductivity detection.

Determination of sodium, potassium, DMEA (dimethylethanolamine), calcium, choline, and magnesium in a saline solution using cation chromatography with direct conductivity detection.

Determination of calcium and magnesium in a dolomite sample using cation chromatography with direct conductivity detection.

Determination of trimethylamine in hydrogen peroxide (31 %) using cation chromatography with direct conductivity detection after inline matrix elimination, inline preconcentration, and inline calibration.

Determination of mono-, di-, and trimethanolamine (MMA, DMA, TMA respectively), in the presence of lithium, sodium, ammonium, potassium, magnesium, cesium, calcium, and strontium using cation chromatography with direct conductivity detection.

Determination of ammonium, magnesium, and calcium in a fertilizer using cation chromatography with directconductivity detection.

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

Determination of ammonium, potassium, magnesium, and calcium in a liquid fertilizer using cation chromatography with direct conductivity detection..

Determination of betaine in the presence of standard cations in an Echinacea product using cation chromatography with direct conductivity detection.

Determination of zinc, sodium, potassium, magnesium, and calcium in an infusion solution using cation chromatography with direct conductivity detection.

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.

Determination of magnesium, manganese, and zinc in a zinc sulfate solution using cation chromatography with direct conductivity detection.

Determination of dimethylamine (DMA), trimethylaminoxide (TMAO), trimethylamine (TMA), putrescine, cadaverine, and histamine in a fish sample using cation chromatography with direct conductivity detection.

Determination of traces of methylamine, isopropylamine diethylethanolamine, and diethylamine in the presence of lithium, sodium, ammonium, potassium, magnesium, and calcium using cation chromatography with direct conductivity detection.

Determination of traces of methylamine, dimethylamine, and trimethylamine in methylpyrrolidone using cation chromatography with direct conductivity detection.

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

Determination of traces of lithium, sodium, ammonium, potassium, calcium, and magnesium in ethanol using cation chromatography with direct conductivity detection after Metrohm Inline Matrix Elimination.

Determination of traces of lutetium, ytterbium, thulium, erbium, terbium, gadolinium, samarium, neodymium, praseodymium, cerium, and lanthanum using cation chromatography with direct conductivity detection.

Determination of traces of gadolinium, samarium, neodymium, cerium, and lanthanum using cation chromatography with direct conductivity detection after Metrohm Inline Filtration.

Determination of choline in infant milk powder using cation chromatography with direct conductivity detection applying Metrohm Inline Dialysis.

Determination of potassium, magnesium, and calcium in biodiesel using cation chromatography with direct conductivity detection applying automated extraction and subsequent Metrohm Inline Dialysis.

Determination of sodium, potassium, magnesium, and calcium in orange juice using cation chromatography with direct conductivity detection applying automated dilution and subsequent Metrohm Inline Ultrafiltration.

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

Determination of traces of ammonium in the presence of sodium, potassium, magnesium, and calcium using cation chromatography with direct conductivity detection.

Determination of copper, zinc, iron(II), and manganese in red wine using cation chromatography with UV/VIS detection after post-column reaction with PAR.

Determination of traces of lutetium, ytterbium, thulium, erbium, terbium, gadolinium, samarium, neodymium, praseodymium, cerium, and lanthanum using cation chromatography with gradient elution and UV/VIS detection after post-column reaction with Arsenazo III.

Determination of hydroxylamine, ethanolamine, triethanolamine, and hydrazine using cation chromatography with direct conductivity detection.

Determination of methylamine in the presence of sodium, ammonium, potassium, magnesium, and calcium using cation chromatography with direct conductivity detection.

Determination of trans-4-methylcyclohexylamine in a pharmaceutical product using cation chromatography with direct conductivity detection.

Determination of tributylamine in a pharmaceutical product (gabapentine) using cation chromatography with direct conductivity detection.

Determination of N-methylpyrrolidone (N-MP) in a pharmaceutical product (Cefepime Hydrochloride) using cation chromatography with direct conductivity detection.

Long-term determination of standard cations with automatic inline eluent preparation using Dosino and Level Control instruments and cation chromatography with direct conductivity detection.

Determination of lysine as well as sodium, ammonium, potassium, and calcium in bulk lysine using cation chromatography with direct conductivity detection.

Determination of sodium, ammonium, potassium, magnesium, and calcium in an ambient aerosol (PM2.5) using aerosol sampling with the PILS (Particle Into Liquid Sampler) and cation chromatography with direct conductivity detection.

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

Determination of sodium and potassium in toothpaste using cation chromatography with direct conductivity detection.

Calibration of lithium, sodium, ammonium, zinc, potassium, magnesium, and calcium using the partial loop technique and cation chromatography with direct conductivity detection. This technique allows a calibration range of 1:100 (e.g. 1 μg/L to 100 μg/L corresponding to 2 μL to 200 μL injected volume) out of 1 calibration solution. Applying the full range of partial loop injection to the samples one calibration covers a sample concentration range of 1 to 10'000 e.g. 2 μL of a 10 mg/L solution corresponds to the highest calibration level (100 μg/L) while 200 μL of a 1 μg/L solution corresponds to the lowest calibration level.

Determination of lithium, sodium, ammonium, zinc, potassium, magnesium, and calcium impurities in syringe filters using cation chromatography with direct conductivity detection.

Determination of Bethanechol chloride and calcium in tablets using cation chromatography with direct conductivity detection.

Determination of Bethanechol Chloride and HPTA (2-hydroxy-propyl-trimethyl ammonium chloride) besides sodium and calcium using cation chromatography with direct conductivity detection.

Determination of strontium and barium in monoethylene glycol using cation chromatography with direct conductivity detection.

Determination of sodium, potassium, iron(II), magnesium and calcium in antifreeze (monoethylene glycol) using cation chromatography with direct conductivity detection. Ascorbic acid reduces iron(III) to iron(II). In this way total iron is determined as iron(II).

Determination of lithium, sodium, ammonium, potassium, calcium, magnesium, and strontium in brine using cation chromatography with direct conductivity detection.

Determination of monoethanolamine (MEA), diethanolamine (DEA), and triethanolamine (TEA) in the presence of lithium, sodium, ammonium, potassium, calcium, and magnesium using cation chromatography with direct conductivity detection.

Determination of monomethylamine (MMA), dimethyl-amine (DMA), and trimethylamine (TMA) in the presence of lithium, sodium, ammonium, potassium, cesium, calcium, and magnesium using cation chromatography with direct conductivity detection.

Determination of monomethylamine (MMA), dimethylamine (DMA), trimethylamine (TMA), monoethanolamine (MEA), diethanolamine (DEA), and triethanolamine (TEA) using cation chromatography with direct conductivity detection.

Determination of benzylamine in a beta blocker (Nebivolol) using cation chromatography with direct conductivity detection. A step gradient for fast elution of the main component is applied.

Determination of dimethylamine in Metformin (N,N-dimethylimidodicarbonimidic diamide, anti-diabetic drug) using cation chromatography with direct conductivity detection.

Determination of lithium, sodium, ammonium, potassium, manganese, calcium, magnesium, strontium, and barium using cation chromatography with direct conductivity detection.

Determination of lithium, sodium, ammonium, potassium, manganese, calcium, magnesium, strontium, and barium in an offshore effluent using cation chromatography with direct conductivity detection.

Determination of magnesium, cadmium, and iron in phosphoric acid using cation chromatography with direct conductivity detection.

Determination of lithium, sodium, ammonium, and monoethanolamine (MEA) using cation chromatography with direct conductivity detection and Metrohm Inline Preconcentration and Inline Calibration.

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.

Eluent preparation on demand (EPOD) is the convenient and flexible way of automatic eluent preparation. The 849 Level Control together with an 800 Dosino equipped with a 50 mL dosing unit are used to dilute an eluent concentrate to the required eluent concentration. The use of eluent concentrates is suitable for any eluent. This facilitates unattended operation of the system over several weeks (see AN S-296 for anion eluent preparation).

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.

Metrohm intelligent Partial Loop Technique (MiPT) is a versatile injection mode in IC. In this application, injection volumes range from 4 to 200 µL (corresponding to 0.5 - 10 mg/L) using the 250 µL loop. Here, the use of 2 and 5 mL Dosing Units are compared.

Water chemistry of the water-steam cycle is crucial for maintaining plant reliability and for ensuring optimal plant operational conditions. Impurities such as corrosion products in ionic, colloidal, or oxide forms are ubiquitous in feedwater, condensate, and reactor coolant. This application shows the determination of sub-ppb levels of Cu, Ni, Zn and standard cations (e.g., Na+, NH4+, Mg2+, Ca2+) in the water-steam cycle of a BWR.

In pressurized water reactors (PWRs), light water is used as primary coolant. Boron (as boric acid) readily absorbs neutrons and is added to the coolant to control reactivity. Lithium hydroxide assures a pH value greater than 7 to prevent corrosion. This application allows to measure sub-ppb levels of zinc, nickel, calcium, and magnesium besides high boric acid and lithium hydroxide concentrations.

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).

In pressurized water reactors (PWRs), light water is used as coolant in the primary side. Boron (as boric acid) is added to the coolant to absorb neutrons, thus controlling reactivity. Lithium hydroxide assures the alkaline pH value to prevent corrosion. This application allows to measure lithium content besides high boric acid concentrations. AN-C-138 shows the respective trace metal determination on the same system setup.

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.

The Metrosep C 6 columns have a higher capacity than those of the Metrosep C 4. The present Application Note describes the exceptional separating efficiency for standard cations with the three Metrosep C 6 column lengths available. The outstanding sodium-ammonia separation is particularly noteworthy.

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.

Metrohm Inline Preconcentration Technique with matrix elimination (MiPCT-ME) is a powerful method that combines preconcentration, matrix elimination, and multilevel calibration. In this Application Note, the methodology is applied to the determination of traces of sodium in addition to 2 mg/L ammonia. The Metrosep C 6 - 250/4.0 column is used for selectivity reasons.

The determination of low ammonium concentrations besides excess sodium is demanding due to the small retention time difference of these two cations. This Application Note shows direct conductivity detection as an ideal means to detect ammonium in a wastewater sample containing 400 mg/L sodium. AN-S-313 shows the analysis of nitrite traces.

Bethanechol is a pharmaceutical compound which is used to treat urinary retention. This API (active pharmaceutical ingredient) can be determined by cation chromatography with direct conductivity detection. A good separation is achieved between bethanechol and its degradation product 2-hydroxy-propyl-trimethyl ammonium (HPTA) and the standard cations. Peak shape and resolution meet the USP requirements for bethanechol.