Applications

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 analytical challenge treated by the present work consists in detecting sub-ppb concentrations of low-molecular-weight amines in the presence of strongly retained cationic drugs by using ion chromatography (IC) with upstream inline coupled-column matrix elimination (CCME). In contrast to direct-injection IC, where the late elution of strongly retained drugs requires eluents with added acetonitrile, the CCME technique uses two preconcentration columns in series. In an «inverse matrix elimination step, cationic drug and target amines are trapped on a high-capacity and a very-high-capacity preconcentration column, respectively. During amine determination, a rinsing solution flushes the drug to waste. This significantly shortens the analysis time and improves sensitivity as well as selectivity. Besides the determination of monomethylamine in Nebivolol hydrochloride discussed here, the CCME technique is a promising tool for detecting further low-molecular-weight amines in a wide range of drugs.

By combining the information from electrochemical and spectroscopic techniques, UV/VIS spectroelectrochemistry (UV/VIS-SEC) allows a comprehensive analysis of electron-transfer processes and complex redox reactions. The anodic oxidation of a N-aryl-D2-pyrazoline derivative was investigated by combining cyclic voltammetry and UV/VIS spectroscopy. In-situ measured UV/VIS absorbance depicted the absorption changes that accompanied the anodic oxidation and could therewith prove the stability of the electrogenerated radical cation. UV/VIS-SEC provides a powerful tool for the in situ study of shorter-lived species, reaction mechanims, and kinetics in a wide variety of electrochemical active organic, inorganic, and biological molecules.

The quantitative determination of the alkaloid nicotine, which is an essential constituent of the tobacco plant, can be carried out by polarography. The quantification limit is less than 0.1 mg/L in the polarographic vessel.

This Bulletin is a supplement to Application Bulletin no. 36 (Half-wave potentials of inorganic substances) in the sense that the half-wave potentials of 100 different organic substances are listed. At the same time the supporting electrolytes used and the limits of determination are given.The various substances are listed in alphabetical order. The most important polarographically active functional groups are taken into consideration. This means that substances for related structures can also be determined polarographically in the same or similar supporting electrolytes, although they may not appear in the list.Unless otherwise stated, the half-wave potentials refer to a temperature of 20 °C, and the potentials are given in volts, measured with a sat. KCI-Ag/AgCl electrode assembly.The determination limits give the smallest concentrations which can be measured without risking serious errors in the results. In all cases, the limit of detection lies below the limit of determination.

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.

Fast IC means short run times and a high sample throughput on columns with a relatively high flow rate and the standard eluent. Mono-, di- and tri-ethanolamine are separated with the Metrosep C 4 - 150/2.0 within 2.5 minutes.

Fast IC means short run times and a high sample throughput on columns with a relatively high flow rate and the standard eluent. Mono-, di- and trimethylamine are separated with the Metrosep C 4 - 150/2.0 within four minutes.

In natural gas production, the removal of contaminants, and in particular acidic gases such as H2S and CO2, is exceptionally important. These acidic gases are removed in the amine wash through chemical treatment with amines or alkanol amines. This application shows a convenient and precise analysis with the separation of various amines and standard cations on a column of the Metrosep C 6 - 250/4.0 type with subsequent direct conductivity detection.

N-methyldiethanolamine and piperazine are used in scrubber solutions, e.g., in the natural gas process. Testing this type of samples by ion chromatography requires a good resolution and the separation of amines from standard cations. The separation is achieved on a Metrosep C 4 - 150/4.0 column applying direct conductivity detection.

Before the liquefaction process of the natural gas, carbonate and hydrogen sulfide need to be removed through a scrubber solution containing piperazine and N-methyl diethanolamine (MDEA). The concentration ratio of the two components is determined by ion chromatography on a Metrosep C 4 - 150/4.0 column applying direct conductivity detection.

Chipped wood and sawdust may be used in production of feed e.g., for ruminants. Melamine, a raw material for resins in wood adhesives, is limited to be used in feed. Therefore, the melamine concentration in sawdust has to be analyzed. Melamine determined after ion chromatographic separation with UV/VIS detection.

Abrasive machining of e.g., metal parts requires a cooling lubricant. Their purpose besides cooling and lubrication is to inhibit corrosion. Amines are added to the emulsion to keep the pH high. In the actual application, DCHA and MDCHA have to be analyzed besides other amine components and inorganic cations. To avoid oil contamination on the IC system, Inline Dialysis is applied. The detection is performed by direct conductivity detection.

The concentrations of toxic, biogenic amines in foods, particularly in fish and wine, are an important quality characteristic. The present Application Note shows the separation of putrescine, cadaverine and histamine in addition to the standard cations. Separation takes place on a Metrosep C Supp 1 - 250/4.0 with Dose-in Gradient; quantification via conductivity detection following sequential suppression.

Atorvastatin is a medication that is used for reducing cholesterol levels. A sensitive and reliable method for TBA detection is required, given that trace amounts of tetrabutylammonium (TBA) are to be found in the presence of atorvastatin and its derivatives. One such method is ion chromatographic separation on the Metrosep C Supp 1 - 250/4.0 with subsequent conductivity detection and sequential suppression.

This Application Note shows the selectivity of the Metrosep C Supp 1 - 250/4.0 column for alkyl and ethanol amines in addition to standard cations under isocratic conditions. Quantification takes place using conductivity detection following sequential suppression.

Meropenem is a beta-lactam antibiotic that is classed among the carbapenems; it suppresses murein biosynthesis and thus the buildup of the bacterial cell wall. Dimethylamine is an important precursor in meropenem synthesis and must therefore be monitored as an impurity. Detection is performed on the Metrosep C Supp 1 - 250/4 column with subsequent conductivity detection after sequential suppression.

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.

Hydrogen peroxide is available in different purity grades depending on its use. High purity H2O2 (electronic grade) requires very low contamination levels, e.g., less than 1 μg/L of trimethylamine (TMA). This application describes the determination of trimethylamine in a high-purity H2O2 solution (30%). Analysis is performed using Inline Preconcentration with Matrix Elimination (MiPCT-ME) applying conductivity detection after sequential cation suppression.

This Application Note presents a walkthrough of an experiment on 4-nitrothiophenol using hyphenated EC-Raman, a combination of Raman spectroscopy and electrochemistry.

Dissolution of urea in glacial acetic acid, and titration with standard 0.1 mol/L trifluoromethanesulfonic acid in acetic acid using isobutyl vinyl ether as a thermometric endpoint indicator.

Weak, organic bases that are soluble in nonaqueous solvents (including nonpolar solvents) are determined in glacial acetic acid using titration with strong acids, e. g., anhydrous perchloric acid or trifluoromethanesulfonic acid. The endpoint of such titrations can be determined thermometrically, insofar as a suitable thermometric endpoint indicator exists. The exceptional suitability of isobutyl vinyl ether (IBVE) as indicator has been demonstrated.

Determination of diethylamine and trimethylamine using cation chromatography with MS detection.

Urea is not a typical analyte for ion chromatography. In combination with MS, however, IC is the method of choice for the trace analysis of urea in ultrapure water. This Application Note shows the determination of urea concentrations in the ppb range using the Metrosep C 6 - 250/4.0 column.

Alendronate, also referred to as alendronic acid, is a biphosphonate used to treat osteoporosis. It is the main ingredient in the tablets and is determined in accordance with the Chinese Pharmacopoeia (2015). Separation takes place in the Metrosep A Supp 4 - 250/4.0 column; direct conductivity detection is used for quantification.

Determination of sulfite, nitrite, nitrate, sulfate, imidodisulfonate, and peroxodisulfate using ion-pair chromatography with conductivity detection after suppression.

Copper is used widely in industrial cooling water systems for its heat transfer properties, although it is susceptible to corrosion. Corrosion can cause a loss of efficiency and eventually a failure of equipment, leading to costly maintenance, replacement, and downtime. Corrosion inhibitors (triazoles) can be added to the water chemistry, which form sparingly soluble protective layers on the surface of the metal. Triazole concentrations must be maintained to protect the copper, which necessitates regular concentration determinations in cooling water. The 2060 IC Process Analyzer with UV/VIS detection is well-suited for this application, able to precisely and reliably measure multiple ionic and UV-active compounds simultaneously in cooling water.

Spectroelectrochemistry is a multi-response technique that provides both electrochemical and spectroscopic information about a chemical system in a single experiment, i.e., it offers information from two different points of view. Spectroelectrochemistry focused on the UV/VIS region is one of the most important combinations because this allows us to obtain not only valuable qualitative information, but also outstanding quantitative results. In this application note, the degradation kinetics for 4-nitrophenol, a known pollutant, were determined using SPELEC.

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.

In 2008, a scandal was discovered in China that melamine was being deliberately added to raw milk. Thousands of young children and infants that consumed formula produced from melamine-tainted milk experienced kidney damage and death. As a result, both daily intake limits and increased monitoring of melamine in dairy products were established globally.Misa (Metrohm Instant SERS Analyzer) provides quick, easy, and robust detection of melamine in a complex food matrix. As a direct test with no additional reagents, Misa’s assay format requires minimal user training, in contrast to standard analytical tests for detecting melamine, including capillary electrophoresis, GC-MS, LC-MS, and immune-based assays.

Determination of hypophosphite, formate, phosphate, adipate, p-nitrobenzoate, and sebacate in ethylene glycol using anion chromatography with conductivity detection after chemical suppression.

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

This Application Note describes the nonaqueous acid-base titration of ketoconazole in accordance with the European Pharmacopoeia. The Solvotrode easyClean was used as the electrode.

The purity of sulfanilamide was determined by means of automatic potentiometric titration using sodium nitrite as the titrant. The solution was spiked with potassium bromide, because bromide ions catalyze diazotization titration.

Nitrilotriacetate (NTA) is a complexing agent that is used in detergents as a water softener. NTA forms complexes with metal ions such as Ca2+, Cu2+ and Fe3+ and thus prevents the formation of lime and its deposits. The NTA content is therefore an important parameter for the quality of detergents and is determined using back titration of an excess of copper nitrate.

Nicotine is a nitrogenous alkaloid that is hazardous to health and is characterized by a very high potential for addiction. The nicotine content in tobacco products must be determined and specified precisely. This Application Note exhibits an easy and straightforward method for nicotine determination in tobacco by non-aqueous titration.Results determined by GC and IC are given as a comparison. In comparison to chromatographic methods, titration is an «absolute method», meaning it is not necessary to calibrate the system prior to the analyses.

Metformin is one the most commonly used drugs for diabetes type 2 belonging to the group of biguanides. This Application Note describes the determination of metformin hydrochloride assay according to USP using acetic anhydride as solvent.

Quaternary ammonium salts are the active ingredients in fabric softener and require accurate determination to assess the cost and the performance of the fabric softener. This Application Note describes the determination of diamidoamine-based quaternary ammonium salts by potentiometric titration.

Quaternary ammonium salts are the active ingredients in fabric softener and require accurate determination to assess the cost and the performance of the fabric softener. This Application Note describes the determination of dialkyl dimethyl quaternary ammonium salts by back titration.

Determination of saccharin, benzamide, and o-toluenesulfonamide in a nickel electroplating bath using RP chromatography with UV detection.

Determination of phenylalanine, aspartame, caffeine, and benzoate in a soft drink using RP chromatography with UV detection.

Determination of thiamine hydrochloride according to USP 28-NF 23 (second supplement) using RP chromatography with UV detection.

Determination of penicillin G potassium and 2-phenyl acetamide in accordance with USP 28-NF 23 (Appendix 2) using RP chromatography and subsequent UV detection. Keyword: Antibiotics

Determination of melamine in milk, diary products, eggs, and egg-based foodstuffs using cation chromatography.

In industrial cooling water systems, copper and its alloys are widely used because of their superior heat transfer properties. These materials are, however, susceptible to corrosion. Azoles are commonly used to protect copper and its alloys from corrosion. These corrosion inhibitors are quantified by ion chromatography with UV/VIS detection.

Determination of coumarin and tartrazine in vodka.

Determination of clothiapine in a pharmaceutical standard.

Quinine can be determined by polarography at the DME using Britton-Robinson buffer at pH = 7.0 as supporting electrolyte.

Thiourea is determined by cathodic stripping voltammetry (CSV) at the HMDE in ammonia buffer at pH 8.9. Chloride in the sample does not interfere with this determination.

The concentration of nitrobenzene in aniline is determined by polarography in an ethanol / acetic acid electrolyte.