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This Bulletin describes titrimetric methods for the determination of cadmium, free sodium hydroxide, sodium carbonate, and total cyanide. The free cyanide can be calculated from the total cyanide and the Cd content.

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.

This Application Note describes a method for the determination of causticizer, carbonate and aluminum oxide in used Bayer process liquors. The method is based on processes that were developed by Watts-Utley and VanDalen-Ward.

Determination of concentrated potassium hydroxide solutions which had been used for the etching of substrates containing silicon.

This Application Note describes the determination of the free and total hydroxide and aluminum oxide content in Bayer process and other aluminate liquors. The method is not subject to interference by carbonate ions. An aliquot of sodium aluminate liquor is titrated with potassium hydrogen carbonate solution to yield the free hydroxide ion content of the liquor.

The Kraft process is the dominant pulping process in the pulp and paper industry with the highest chemical recovery efficiency. In order to run each part of the papermaking process optimally, constant quality checks and analyses should be performed. This Process Application Note illustrates the straightforward online analysis of alkali (active, effective, total titratable alkali (TTA)), carbonate, hydroxide, sulfide and the causticizing degree (CE%) in pulping liquors using a 2060 Process Analyzer from Metrohm Process Analytics.

The chemicals used in the manufacture of semiconductors must exhibit an exceptional purity, because even traces of contaminants have a negative effect on electrical properties. For the manufacture of printed circuit boards, the light-sensitive photoresist applied to the substrate (wafer) is exposed to light at defined areas with the aid of a photo template and then developed in a chemical reaction. The developer contains 2.38 to 2.62% tetramethylammonium hydroxide (TMAH) and ensures that the exposed areas can be readily separated from the substrate. The monitoring of the TMAH concentration in the developer solution takes place with a process analyzer from Metrohm Applikon that is configured specially for titration. In addition to this, the analyzer helps with the mixing of the TMAH solutions.

The Bayer Process is the method used to refine alumina from bauxite ore, as smelting aluminum directly from alumina is much more cost- and energy-effective. In this process, "aluminate liquors" are created by digesting the crushed bauxite with CaO and NaOH at high temperatures. Additionally, the CaO causticizes carbonate which forms in the alkaline solution from organic degradation and CO2 absorption from the atmosphere. Contaminations are removed at various steps in the process, and the liquor is filtered from the alumina crystals before it is recycled back to the digestion step. Before the spent liquor can be reused, a determination of the concentrations of the total hydroxyl (“caustic”), carbonate, and alumina values is required. These parameters can be determined quickly via thermometric titration with the 2035 Process Analyzer.

Determination of hydroxide and carbonate in alkaline plating baths by potentiometric titration with HCl using the combined glass electrode.

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

Electroplating processes are used in several different industry sectors to protect the surface quality of various products against corrosion or abrasion and significantly improve their working life. It is essential to check the bath composition on a regular basis to ensure that the process is operating correctly. Typical examples of electroplating baths include alkaline degreasing baths or acidic or alkaline baths containing metals e.g. copper, nickel, or chromium, or components like chloride and cyanide. It is crucial that the chosen analysis technique fulfills high safety standards for these kinds of analyses and produces reliable results. The OMNIS Sample Robot system automatically pipettes and analyzes aggressive electroplating bath samples on different workstations, increasing the safety in the lab. This provides more reliable results in comparison to manual titration and is more time efficient as different parameters can be analyzed in parallel.

This Application Note compares the OMNIS Titrator and 888 Titrando for determinations of nitric acid, phosphoric acid, and acetic acid in an aluminum etching bath, as well as the determination of tetramethylammonium hydroxide (TMAH). Identical analysis parameters were used, showing that OMNIS delivers results on par or even better than with other established titration systems.

The amine value is an important parameter and quality indicator to determine in chemical processes and pharmaceuticals. This Application Note presents the nonaqueous perchloric acid titration of triethanolamine.

Chlorine and caustic soda are used as feedstock materials in myriad production processes for several markets including pulp and paper, petrochem, and pharma. The chlor-alkali process, accounting for 95% of production, depends on the electrolysis of brine, which first requires several steps of purification. This white paper describes the reasoning and benefits for online and inline process analysis over conventional methods for the production of these basic chemicals.

This white paper summarizes the steps involved in converting an existing manual titration procedure to semi-automated or automated titration procedures. It discusses topics such as selecting the right electrode and titration mode. For a better understanding, the discussion topics are illustrated with three examples.

The objective of validation of an analytical procedure is to demonstrate that it is suitable for its intended purpose. Recommendations for the validation of analytical methods can be found in ICH Guidance Q2(R1) Validation of Analytical Procedures: Text and Methodology and in USP General Chapter <1225> Validation of Compendial Procedures. The goal of this white paper is to provide some recommendations for the validation of titration methods.