Aplicações

Hydroxyl is an important functional group and knowledge of its content is required in many intermediate and end-use products such as polyols, resins, lacquer raw materials and fats (petroleum industry). The test method to be described determines primary and secondary hydroxyl groups. The hydroxyl number is defined as the mg of KOH equivalent to the hydroxyl content of 1 g of sample.The most frequently described method for determining the hydroxyl number is the conversion with acetic anhydride in pyridine with subsequent titration of the acetic acid released: H3C-CO-O-CO-CH3 + R-OH -> R-O-CO-CH3 + CH3COOH. However, this method suffers from the following drawbacks: - The sample must be boiled under reflux for 1 h (long reaction time and laborious, expensive sample handling) - The method cannot be automated - Small hydroxyl numbers cannot be determined exactly - Pyridine has to be used, which is both toxic and foul-smellingBoth standards, ASTM E1899-08 and DIN 53240-2, offer alternative methods that do not require manual sample preparation and therefore can be fully automated: The method suggested in ASTM E1899-08 is based on the reaction of the hydroxyl groups attached to primary and secondary carbon atoms with excess toluene-4-sulfonyl-isocyanate (TSI) to form an acidic carbamate. The latter can then be titrated in a non-aqueous medium with the strong base tetrabutyl- ammonium hydroxide (TBAOH). The method suggested in DIN 53240-2 is based on the catalyzed acetylation of the hydroxyl group. After hydrolysis of the intermediate, the remaining acetic acid is titrated in a non-aqueous medium with alcoholic KOH solution. The present work demonstrates and discusses an easy way to determine the hydroxyl number according to ASTM E1899-08 or DIN 53240-2 with a fully automated titrimetric system for a great variety of industrial oil samples.

The presence of excessive water in plastics adversely affects the performance of polymeric goods which is why water determination is of crucial importance. This article describes the accurate and straightforward determination of the water content using the Karl Fischer Oven Method in ten different plastic types that are not amenable to direct Karl Fischer titration. The experiments revealed that besides the determination of the oven temperature, sample preparation is one of the most important steps of the analysis, especially in case of hygroscopic plastic samples.

The Combustion IC system presented allows the automated determination of organic halogen and sulfur compounds in all flammable samples. Both combustion digestion, which is automatically controlled with a flame sensor, and the professional Liquid Handling guarantee highest precision and trueness. This poster describes the determination of the halogen and sulfur content in a certified polymer standard, a coal reference material as well as in latex and vinyl gloves.

Indication of the titration endpoint of the weakly alkaline or weakly acidic terminal groups in non-aqueous solution is frequently not easy. An improvement is possible by using a suitable titrant (TBAH = tetrabutylammonium hydroxide for terminal carboxyl groups; perchloric acid for terminal amino groups). An improvement in the evaluation can also be achieved by choosing benzyl alcohol as the solvent. The choice of electrode combination and the measuring setup is also important. Differential potentiometry using the three-electrode technique results in a great improvement in titrations in poorly conducting solutions. Noisy signals are eliminated.

This Application Bulletin describes a simple polarographic method to determine monomeric styrene in polymers. The limit of determination lies at 5 mg/L. Before the determination, styrene is converted to the electrochemically active pseudonitrosite using sodium nitrite.

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.

Os poliuretanos são um dos tipos de plástico mais comumente usados. Eles são produzidos pela reação de polióis brutos com isocianatos. Dependendo do material de partida pode ser obtida uma grande variedade de plásticos. A determinação do índice de acidez, do índice de hidroxila e do teor de isocianato desempenha um papel importante na análise de matérias-primas para plásticos. O índice ácido da matéria-prima poliol é geralmente usado no controle de qualidade para garantir a uniformidade entre lotes. Além disso, é usado como fator de correção para calcular o verdadeiro número de hidroxila. Neste Boletim de Aplicação é descrita a determinação do índice de acidez de acordo com ASTM D4662 e ASTM D7253. Uma matéria-prima para poliuretanos são os polióis. Os polióis contêm vários grupos hidroxila. Portanto, o número de hidroxila de uma matéria-prima se correlaciona diretamente com a quantidade de polióis presentes e é, portanto, um importante parâmetro de controle de qualidade. Neste Boletim de Aplicação é descrita a determinação do índice de hidroxila de acordo com ASTM E1899 e DIN 53240-3. Como os polióis reagem estequiometricamente com os isocianatos, o conhecimento do teor de isocianato é um importante parâmetro de qualidade para a produção de poliuretanos. Neste documento é descrita a determinação de acordo com EN ISO 14896 método A, ASTM D5155 método A e ASTM D2572.

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.

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.

O sistema de titulação apresentado pode ser utilizado para a determinação totalmente automatizada do número de hidroxila (HN) de acordo com ASTM E1899 e EN ISO 4629-2. O método permite a determinação de polióis e oxoóleos sem ferver sob refluxo ou outra preparação de amostra e é, portanto, um grande benefício para laboratórios que precisam lidar com um alto rendimento de amostras. As normas EN 15168 e DIN 53240-3 baseiam-se no mesmo método de análise da ASTM E1899.