Filtro de Aplicações

The thermometric titration method presented here permits a simple and direct determination of the total acid number (TAN) in petroleum products. It is an invaluable alternative to current manual and potentiometric methods. Thermometric titration uses a maintenance-free temperature sensor that does not require rehydration and is free of fouling and matrix effects. The procedure requires minimal sample preparation. Results agree closely with those from the potentiometric titrimetric procedure according to ASTM D664, but the thermometric titration method is far superior in terms of reproducibility and speed of analysis, with determinations being complete in approximately one minute.

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

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.

Agriculture at significant scale without fertilizers is no longer possible in the modern world. To grow a sufficient amount of produce for nearly 8 billion people as well as for domesticated animals and industrial uses, fertilizers of different nutrient compositions are available to cater to the unique needs of various soil types. Information on the fertilizer’s composition (e.g., total nitrogen, phosphorus, and potassium) is available to help select the ideal fertilizer for a specific soil. Conventionally these constituents are determined either gravimetrically (e.g., phosphorus, potassium, or sulfate) or with ICP-OES (e.g., phosphorus or potassium). These methods either have the disadvantages of long analysis times combined with laborious sample preparation (gravimetry), or require expensive instrumentation with high running costs (ICP-OES). This White Paper elaborates how thermometric titration is a fast and inexpensive alternative method to provide information on the content of various nutrients in different fertilizers.

Phosphorus is a primary macronutrient for plants and is a constituent of DNA and adenosine triphosphate (ATP), which is involved in many biological processes requiring energy. In fertilizers, phosphorus is present in the form of phosphate, as the most accessible form of phosphorus for plants is dihydrogen phosphate. Knowledge of the phosphorus content helps to select the right fertilizer for the plants. Traditionally, phosphate is determined gravimetrically (a time consuming procedure) or spectrophotometrically (expensive instrumentation). In this Application Note, an alternative method is presented, where phosphate is determined by a precipitation titration with magnesium. Various solid and liquid NPK fertilizers with phosphorus contents between 6.5 and 17% were analyzed. The analysis by thermometric titration requires no sample preparation in case of liquid NPK fertilizers and only minimal sample preparation in case of solid NPK fertilizers. One determination takes about 5 minutes.

Sulfur is a secondary macronutrient for plants and is essential for chloroplast growth and function. In fertilizers, sulfur is usually provided in the form of sulfate. Traditionally the sulfate content is determined gravimetrically by precipitation with barium. The drawback of this method is that it requires numerous time consuming and laborious analysis steps. In this Application Note, an alternative method is presented, where sulfate is determined by a precipitation titration with barium chloride. Various solid and liquid NPK fertilizers with sulfur contents between 1 and 8% were analyzed. The analysis of sulfate in fertilizers by thermometric titration requires no sample preparation at all for liquid NPK fertilizers, and only minimal sample preparation for solid NPK fertilizers. One determination takes about 3 minutes only. To increase the sensitivity of the method, the samples are spiked with a standard sulfuric acid solution, which is then considered when calculating the result.

Metrohm has partnered with industry leaders to develop an alternative standard for the measurement of acid number (AN) in crude oil and petroleum products to overcome shortcomings in the current method (ASTM D664). This new standard method (ASTM D8045) describes the use of thermometric catalytic titration for this analysis. Results agree closely with those from ASTM D664, but the thermometric catalytic titration method is far superior in terms of reproducibility and speed of analysis, with determinations being complete in one minute.Solvent usage is much less compared to older methods, saving on waste disposal cost. Comparison studies show very close data correlation between ASTM D8045 and traditional potentiometric AN titration methods making implementation into a refinery with historic data practical.

Samples of shredded, grated, or sliced cheese are dispersed with a high-speed disintegrator in a solution of trichloroacetic acid, which denatures protein and assists in the liberation of all sodium from the matrix. Toluene is added in a second step of the dispersion process to assist in the solubilization of fat. Ammonium fluoride solution is then added, and the sodium titrated with a titrant comprising 0.5 mol/L Al(NO3)3 and 1.1 mol/L KNO3 to an exothermic endpoint. Na+ + 2K+ + Al3+ + 6F- ↔ NaK2AlF6 ↓ In this determination, ammonium fluoride (NH4F) has been found to give sharper endpoints than ammonium bifluoride (NH4F ∙HF). In addition to this application note, you can find more information on thermometric sodium determination in foods in our application video available on YouTube: https://youtu.be/lnCp9jBxoEs

Hydrogen peroxide solutions can be determined through thermometric endpoint titration (TET) using iodometry. Iodide is oxidized to become iodine, which is then titrated with a standard thiosulfate solution in an exothermic reaction.

This Application Note describes the determination of aluminum in samples containing silicon dioxide using thermometric titration and EDTA as the titrant. Excess EDTA is titrated with a Cu2+ solution of known concentration. The initial, uncomplexed Cu2+ ions react immediately with the H2O2 present in the solution, leading to a recognizable sudden increase in temperature.