Applikationer

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.

Carbonyl compounds (CC) occur in many products, such as bio-oils and fuels, cyclic and acyclic solvents, flavors and mineral oils. Carbonyl compounds can be responsible for the instability of these products during storage or processing. Especially pyrolysis bio-oils are known to cause issues during storage, handling and upgrading. This bulletin describes an aqueous and a non-aqueous analytical titration method for the determination of carbonyl compounds by potentiometric titration.

The bromine number and bromine index are important quality control parameters for the determination of aliphatic C=Cdouble bonds in petroleum products. Both indices provide information on the content of substances that react withbromine. The difference between the two indices is that the bromine number indicates the consumption of bromine in gfor 100 g sample and the bromine index in mg for 100 g sample.This Application Bulletin describes the determination of the bromine number according to ASTM D1159, ISO 3839, BS2000-130, IP 130, GB/T 11135 and DIN-51774-1. The bromine index determination for aliphatic hydrocarbons is described according to ASTM D2710, IP 299, GB/T 11136 and DIN 51774-2. For aromatic hydrocarbons the determination of the bromine index is described according to ASTM D5776 and SH/T 1767. UOP 304 is not recommended for the determination of the bromine number or bromine index because its titration solvent contains mercuric chloride.

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.

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

Determination of fluoride, chloride, bromide and sulfate in residual solvent using combustion digestion as sample preparation and subsequent anion chromatography with conductivity detection following sequential suppression. The analysis is significant for use in dividing waste products into non-halogenated and halogenated solvents.Keyword: pyrohydrolysis

This application describes the determination of fluoride, chloride, bromide and sulfur (as sulfate) in an ethanol standard solution with halo organic (4-halogen benzoic acids; F, Cl and Br) and sulfur organic compounds (3-(Cyclohexylamino)-1-propanesulfonic acid) by means of Metrohm Combustion Ion Chromatography with flame sensor and Inline Matrix Elimination.Keyword: pyrohydrolysis

Cyclohexane is an important organic solvent. Recycled cyclohexane must be tested for trace substances, e.g., chloride and sulfate. Metrohm Combustion Ion Chromatography with flame sensor and Inline Matrix Elimination is the method of choice.Keyword: pyrohydrolysis

Cellulose ester foils are produced using chlorinated solvents. The residual amount of the solvent used in production evaporates within a few days in ambient conditions. The residual solvent is determined by combustion IC, through the conversion of organically bound chlorine to chloride by pyrohydrolysis. The final product needs to be free of all chlorinated solvents. Therefore, critical contents of such compounds can be detected in quality control analysis. Application of MiPT in this study has enabled an automated and precise calibration out of a single standard.

A corrosion inhibitor is a substance that reduces the corrosion rate of a metal. A corrosion inhibitor is usually added in a small concentration to the corrosive environment. This application note shows how Metrohm Autolab instruments can be used to check the quality of inhibitors.

The kinetic and mass transfer parameters of the electro-oxidation reaction of TEMPO were measured using the TSC Surface measuring cell for the Autolab Microcell HC system. The cell allows the study of electrochemical processes in liquid electrolytes in a three electrode configuration under temperature control.

In this application note, the advantage of recording the raw time domain data for each individual frequency during an electrochemical impedance measurement is described.

The water content of ethylene dichloride is determined according to Karl Fischer. As the sample may contain free chlorine, which interferes with the determination, separate KF reagents have to be used.

The water content of piperidine and piperazine is determined according to Karl Fischer using a buffered solvent mixture.

The water content in methylcyclohexane is determined by coulometric Karl Fischer titration.

Determination of acetate, formate, chloride, bromide, and sulfate in toluene using anion chromatography with direct conductivity detection.

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

The purity of a recovered solvent (dichlormethane/methylene chloride) and two of its most important contaminants (methanol and water) are monitored with NIR spectroscopy.

Near-infrared spectroscopy (NIRS) can determine water content in PGME (propylene glycol monomethyl ether) within seconds as shown in this Application Note.

Determination of L-lactide, citrate, and lactate in an acetone solution using ion-exclusion chromatography with direct conductivity detection.

In the HPPO – hydrogen peroxide to propylene oxide – process for propylene oxide production, hydrogen peroxide is analyzed using a complexing agent and a colorimetric measurement with dipping probe. Due to the hazardous environment, the online analyzer fulfills EU Directives 94/9/EC (ATEX95) and is certified for zone1 and zone2 areas.

In the cumene process, phenol and acetone are produced from benzene and propylene. For a successful process control, it is crucial to monitor the sulfuric acid concentration, which impacts the acid-catalyzed cleavage of cumene hydroperoxide to yield phenol and acetone. This Process Application Note describes the online analysis of sulfuric acid using titration. In such hazardous environments, the analyzer can be ex-proof or located in an ex-proof shelter.

This Process Application Note presents a method to accurately monitor low levels of moisture in tetrahydrofuran (THF) in «real-time» safely, reliably, and optimally with a 2060 The NIR Analyzer from Metrohm Process Analytics. Due to the hazardous and hygroscopic nature of THF, a single explosion-proof inline process analyzer is the preferred solution for industries to reduce chemical treatment, improve product quality, and increase profits.

Many electrochemical methods have been developed but are traditionally limited to aqueous media. Raman spectroelectrochemistry in organic solutions is an interesting alternative, but developing new EC-SERS procedures is still required. This Application Note demonstrates that the electrochemical activation of gold and silver electrodes enables the detection of dyes and pesticides in organic media.

This Application Note describes the rapid and non-destructive identification of conventional organic solvents using hand-held Raman spectrometers. Measurements with the handheld Raman spectrometer Mira M-1 require no sample preparation and provide immediate and unambiguous results.

Determination of hexafluorophosphate in an ionic liquid BMIHFP (1-butyl-3-methylimidazolium hexafluorophosphate, >97%) using anion chromatography with conductivity detection after chemical suppression.

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

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

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

The hydroxyl number is an important sum parameter for quantifying the presence of hydroxyl groups in a chemical substance. As a key quality parameter, it is regularly determined in various polymers like resins, paints, polyesterols, fats and solvents. Unlinke other standards, ASTM E1899 works pyridine-free and without refluxing at elevated temperatures for a longer time. It is performed at room temperature, requires only a small sample size, is applicable to extremely low hydroxyl numbers (<1 mg KOH/g sample) and can be performed fully automatically. This Application Note describes the potentiometric determination of the hydroxyl number in 1-octanol and polyethylene glycol according to ASTM E1899, EN 15168 and DIN 53240-3. Using the OMNIS DIS-Cover technique all sample preparation steps can be fully automated. Moreover, the use of an OMNIS Sample Robot allows parallel analysis of multiple samples. The average time per analysis for one sample is thus reduced from approximately 24 min to 12 min., increasing productivity in the laboratory considerably.

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.

Carbonyl compounds occur in many products such as bio-oils and fuels, solvents, flavors, and mineral oils. Carbonyl compounds are often prone to oxidation and thus their content has an influence on stability during storage or processing. Especially for pyrolysis bio-oils, stability issues are observed during storage, handling, and upgrading.Oils are dissolved in isopropanol. After a reaction with the hydroxylamine hydrochloride at 50 °C, a fast and accurate determination by potentiometric titration using the dSolvotrode and tetra-n-butylammonium hydroxide as titrant is performed.

Denatured fuel ethanol may contain additives such as corrosion inhibitors and detergents as well as contaminants from manufacturing that can affect the acidity of produced ethanol fuel. An increased acid content in solvents could lead to a variety of problems like a shorter storage stability or chemical corrosion. Using the Optrode with phenolphthalein as indicator, the acidity is determined as acetic acid by titration with sodium hydroxide as titrant.

Denatured fuel ethanol may contain additives such as corrosion inhibitors and detergents as well as contaminants from manufacturing that can affect the acidity of produced ethanol fuel. An increased acid content in solvents could lead to a variety of problems like a shorter storage stability or chemical corrosion.Using the dSolvotrode for indication, the acidity is determined as acetic acid by titration with sodium hydroxide as titrant.

Corrosion of metallic components is an inherent problem for engines, because metals naturally tend to oxidize in the presence of water and/or acids. Increased acid content is indicated by a low pH value, and could lead to a variety of problems like a shorter storage life (stability) or a reduced buffer capacity of the used engine coolant or antirust.In this Application Note, engine coolants or antirust samples are dissolved in water, and the pH measurement using the Profitrode is carried out according to ASTM D1287.

The presence of acidic components in volatile solvents could be a result of contamination, decomposition during storage, distribution or manufacture. An increased acid content in solvents could lead to a variety of problems like shorter storage stability or chemical corrosion. Using the Optrode for indication, the acidity is determined by photometric titration with sodium hydroxide as titrant and phenolphthalein as indicator. If the volatile solvent is water soluble, it is dissolved in deionized water, if not, it is dissolved in carbon-dioxide free ethanol.

The bromine index is an important parameter for the determination of aliphatic C=C double bonds in petroleum hydrocarbons. For the titration, a solvent mixture of glacial acetic acid, methanol, and dichloromethane is usually used.In this Application Note, the chlorinated solvent in the solvent mixture was replaced with toluene, resulting in a more environmentally beneficial method in comparison to ASTM D2710 and IP 299.

The bromine index is an important quality control parameter for the determination of aliphatic C=C double bonds in aromatic hydrocarbons and is thus a measure for the presence of aliphatic unsaturation in these materials. In situ generated bromine reacts with the aliphatic double bonds. When the titration is finished an excess of free bromine causes a sudden change in the measured potential thus indicating the equivalence point.

Ethanol, bio-ethanol and biofuel (E85) are increasingly used as substitutes for petroleum-based fuels. During storage, they often come into contact with metallic substrates or surfaces, e.g., in barrels, tanks, or other containers. Excessive concentrations of ions in the stored fuel promotes corrosion. Monitoring the total concentration of the ions present in the fuel matrix should be the first step of an effective anti-corrosion strategy.An easy, fast, and cost-effective method to determine the total amount of ions is by measuring the electrical conductivity according to DIN 15938.

This Application Note shows the automatic pH adjustment of a mixture of acetonitrile, water and amine using a Metrohm titrator.

Titration is an accurate and precise method that can be used to determine the pyrophosphate content in aqueous products. The OMNIS Titrator equipped with a dUnitrode delivers reliable determinations.

Zn and Pb are determined by anodic stripping voltammetry (ASV) in acetate buffer at pH 4.6.

Iron can be determined in ethanol by adsorptive stripping voltammetry (AdSV) at the HMDE. PIPES buffer is used as supporting electrolyte and catechol as complexing agent at a pH value of 7.0.

This polarographic method uses the Multi-Mode Electrode Pro for simultaneous detection of carbonyl impurities in alcohols, ensuring high product quality and stability.

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

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

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