Uygulamalar

Tartaric Sulfuric Anodizing (TSA) is an established technique for corrosion protection in the aerospace industry. It is an alternative to the environmentally harmful chromic anodizing process. As such, a method to monitor the levels of sulfuric acid and tartaric acid in TSA plating baths is required. Potentiometric titration methods have been developed, and are widely used across the industry. Their disadvantage is that two titrations with different electrodes and solvents are required.In this Application Note, an alternative method is presented, where the concentration of both acids is determined in sequence using a thermometric sensor. Compared to potentiometric titration, thermometric titration is faster and more convenient (no sensor maintenance required). On a fully automated system, the determination of both parameters takes about 7 minutes.

This bulletin discusses automated determination of sodium in milk products available to the public using a 859 Titrotherm and a 814 USB Sample Processor. The sodium content of milk can be rapidly and easily titrated thermometrically with a standard solution of Al3+ as titrant. Thermometric titrations are conducted under conditions of constant titrant addition rate. The molarity of the titrant is computed automatically in tiamoTM (software) with the SLO command. Results are reported as mg Na/100 mL. In addition to this application bulletin, you can find more information on thermometric sodium determination in foods in our application video available on YouTube:https://youtu.be/lnCp9jBxoEs

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.

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

In an acidic solution (containing NH4F * HF, Al(NO3)3 / KNO3) sodium forms NaK2AlF6 which precipitates in an exothermic solution, enabling analysis by thermometric titration. Several foods were analyzed, namely bouillon, gravy, tomato ketchup, corn chips, pretzel sticks as well as crackers. The reproducibility of the results was good. After weighing in and adding solutions, samples were crushed with a polytron to ensure homogeneity in the measuring solution. Relative standard deviations were between 0.08% and 3.75%. In addition to this application bulletin, you can find more information on thermometric sodium determination in foods in our application video available on YouTube:https://youtu.be/lnCp9jBxoEs

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.

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.

Automated thermometric titration of the nickel content of electroless nickel plating solutions. The determination is suitable for fully automated titration employing a 814 Sample Processor.

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.

Boric acid is used in many primary circuits of nuclear power plants, in nickel plating baths, and in the production of optical glasses. Furthermore, boron compounds are found in washing powders and fertilizers. This bulletin describes the potentiometric and thermometric determination of boric acid. The determination also covers further boron compounds, when acidic digestion is applied.

This Application Note describes in detail how to determine the blank value and the titer for thermometric titrations using tiamo™.

Online acid number analysis in various oil products is possible with thermometric catalytic titration according to ASTM D8045 using the 2060 TI Ex Proof Process Analyzer.

Sulfate can be rapidly and easily titrated thermometrically using a standard solution of Ba2+ as titrant. In industry, the widespread procedure is applied to the determination of sulfate in wet-process phosphoric acid.

Sulfate can be rapidly and easily titrated thermometrically using a standard solution of Ba2+ as titrant. In industry, the widespread procedure is applied to the determination of sulfate in wet-process phosphoric acid. This bulletin deals with the determination of sulfate in granular fertilizers such as MAP (monoammonium phosphate), DAP (diammonium phosphate) and TSP (triple superphosphate). Results are reported as percentage of elemental sulfur, %S.

This bulletin deals with the automated determination of calcium and magnesium in commercially available finished milk products using a 859 Titrotherm and a 814 USB Sample Processor. Calcium and magnesium in milk can be rapidly and easily titrated thermometrically using a standard solution of Na4EDTA as titrant.Thermometric titrations are conducted under conditions of constant titrant addition rate. The molarity of the titrant is computed automatically in tiamo (software) using the SLO command. Results are reported as mg Ca and Mg/100 mL.

In titration, the titrant reacts with the analyte either exothermically (gives off heat) or endothermically (absorbs heat). The Thermoprobe measures the temperature change during titration. When all of the analyte has reacted with the titrant, the temperature of the solution will change, and the endpoint of the titration is indicated by an inflection in the temperature curve. Catalytically enhanced titrations using paraformaldehyde as catalyst are based on the endothermic hydrolysis of the paraformaldehyde in the presence of excess hydroxide ions. Edible oils are dissolved in a mixture of toluene and 2-propanol (1:1) and titrated with standardized TBAH (0.01 mol/L) in 2-propanol to a catalytically enhanced endpoint.

Phosphate can be rapidly and easily titrated thermometrically using a standard solution of Mg2+ as titrant. The phosphate-containing solution is basified and buffered with NH3/NH4Cl solution before titration. The formation of insoluble MgNH4PO4 is exothermic. The method is a titrimetric adaptation of a classical gravimetric procedure. This bulletin deals with the determination of phosphate in phosphoric acid and granular fertilizers such as MAP (monoammonium phosphate), DAP (diammonium phosphate) and TSP (triple superphosphate). Results are reported as percentage of P and P2O5.

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.

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.

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.

This bulletin deals with the automated determination of mixtures of HNO3, HF and H2SiF6 in the range of approximately 200-600 g/L HNO3, 50-160 g/L HF, and 0-185 g/L H2SiF6 using thermometric titration.Etch acid mixtures containing HNO3, HF and H2SiF6 from the etching of silicon substrates can be analyzed in a sequence of two determinations using the 859 Titrotherm. The first determination involves a direct titration with standard c(NaOH) = 2 mol/L, followed by a back titration with c(HCl) = 2 mol/L. This determination yields the H2SiF6 content plus a value for the combined (HNO3+HF) contents. The second determination consists of a titration with c(Al3+) = 0.5 mol/L to determine the HF content. For freshly made up mixtures of HNO3 and HF containing no H2SiF6, a linked two-titration sequence is employed. Results from the two determinations are used by tiamoTM to yield individual results for HNO3, HF and H2SiF6.

Thermometric titration can solve application problems that potentiometry cannot solve at all, or at least not satisfactorily.

Thermometric titration is used for the determination of hydrochloric acid and phosphoric acid in acid mixtures. Two endpoints appear on the titration curve that are used for the determination of the two acids.

Thermometric titration is used to determine hydrofluoric acid and nitric acid in etching baths containing ethanol and acetonitrile. Two endpoints appear on the titration curve that are used individually for the quantification of the respective acid.

Thermometric titration can be used for the ready determination of sulfuric acid and phosphoric acid in acid mixtures. An endpoint for each acid appears on the titration curve that can be used to quantify the respective acid.

Thermometric titration is used to determine hydrochloric acid and hydrofluoric acid (hydrogen fluoride) in etching baths containing ethanol and acetonitrile. Two endpoints appear on the titration curve that are used individually for the quantification of the respective acid.

Thermometric titration is used for the determination of hydrochloric acid and nitric acid in acid baths. The entire acid content is titrated with caustic soda in the initial titration; the hydrochloric acid content is then determined in a second titration using silver nitrate solution.

Many refiners look at discounted opportunity crudes as a means to improve their margin spread. The varieties of these cheap crude oils on the market are growing in number, but they have hidden risks for the purchaser caused by factors such as high naphthenic acid and sulfur content. Sulfur compounds and naphthenic acids are among the substances that contribute to the corrosive nature of crude oils and petroleum products. This is why the risk of corrosion is increased when processing crude oils with high naphthenic acid and sulfur content. The refiner must balance the cost benefit versus the risk and the cost of corrosion control when processing these crudes. A reliable acid number determination is a crucial part of corrosion control. Guest authors Bert Thakkar, Bryce McGarvey, and Colette McGarvey of Imperial Oil and Larry Tucker and Lori Carey of Metrohm USA were involved in the development of the new ASTM Method D8045 for acid number determination. Here, they report on the method and how it came to be.

The phosphoric acid content can be easily titrated with a standardized solution of 2 mol/L NaOH. The interfering calcium content in phosphoric fertilizer can be eliminated by adding a saturated oxalate solution.

This Bulletin describes potentiometric titration methods for the determination of the acidity in milk and yoghurt according to DIN 10316, ISO/TS 11869, IDF/RM 150, ISO 6091 and IDF 86, the chloride content in milk, butter and cheese according to EN ISO 5943, IDF 88, ISO 15648, IDF 179, ISO 21422, and IDF 242. Additionally the determination of the sodium content in milk using the thermometric titration is described. The determination of the oxidation stability of butter in accordance to AOCS Cd 12b-92, ISO 6886 and GB/T 21121 as well as the determination of lactose in lactose free milk by ion chromatography is also described.For the determination of the pH value in dairy products see Application Bulletin AB-086 and for the determination of calcium and magnesium see Application Bulletin AB-235.

Potassium is a primary macronutrient for plants, as it plays an important role in water regulation as well as plant growth. In NPK fertilizers, potassium is present besides nitrogen and phosphorus, which are the other two primary macronutrients. Knowing the quality and content of a NPK fertilizer allows an optimal fertilizer management for a planned culture, saving costs and increasing profitability.Traditionally potassium is determined gravimetrically or by flame photometry. In this Application Note, an alternative method is presented, where potassium is determined a precipitation titration. Various solid and liquid NPK fertilizers with potassium contents between 10 and 27% were analyzed. After the removal of any present ammonia, the potassium can be determined reliably in about 5 minutes.

Following the addition of caustic soda, hexafluorosilic acid can be determined through back titration of excess hydroxide with hydrochloric acid. Hydrofluoric acid (hydrogen fluoride) is determined by precipitation with aluminum in the presence of sodium and potassium ions. Nitric acid is determined by subtracting the equivalence concentrations of hexafluorosilic acid and hydrofluoric acid from the total acid concentration.

This Application Note looks at the determination of ferrous ion in acidic solutions from approximately 0.25 g/L by thermometric titration with ceric titrant. The exothermic oxidation reaction shows a sharp endpoint that is detected using the Thermoprobe as a sensitive temperature sensor.

This Application Note describes the determination of total sodium content in canned fish products using thermometric titration. 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

This Application Note deals with the determination of ferric ion in acidic and copper-free solutions using thermometric titration. The ferric ion is reduced by iodide. The released iodine reacts exothermically when titrated with thiosulfate solution. The endpoint is determined through temperature plotting by the temperature sensor Thermoprobe.

Sodium can be determined thermometrically in cheese without sample preparation and addition of additives. A homogenizer is responsible for distribution and stirring. 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

Iron sucrose injections are used during the treatment of iron deficiency anemia. They contain a mixture of ferric iron (Fe3+) and ferrous iron (Fe2+). Ferrous iron content may be determined by subtracting the ferric iron content from the total determined iron content. Yet, this increases the measurement error due to error propagation. Alternative determination of iron(II) with cerium(IV) by potentiometric titration may be hampered, as the equivalence point cannot be determined unequivocally. Determination by thermometric titration is a more robust and therefore more reliable alternative, as this method is unaffected by the sample matrix. Here, the endpoint of the titration is indicated by a fast responding thermometric sensor. Endpoint detection is further improved by spiking the sample with 0.2% ammonium iron(II) sulfate (FAS), increasing the reliability of the determination. Compared to potentiometric titration, thermometric titration is faster and more convenient as no sensor maintenance is required. One determination takes about 2–3 minutes.

Automated mixing of a suspension and a solvent in a 50 mL dosing unit can be used to add a well-defined amount of a suspension-solvent mixture to a sample solution without clogging the dosing unit and tubing by the undiluted suspension.The method is explained by means of the TAN determination of a petroleum sample using thermometric titration. For a better endpoint recognition, small amounts of a paraformaldehyde-solvent suspension are added (catalyzed endpoint thermometric titration).

Thermometric titration can determine the total acid number (TAN) of various crude oil products according to ASTM D8045 without requiring any sensor maintenance.

Standardization of ~1mol/L tetrasodium EDTA solutions for thermometric complexometric analysis.

Standardization of disodium dimethylglyoximate by thermometric titration with standard Ni(II) solution.

Determination of bicarbonate and carbonate in a mixture by sequential thermometric titrations.

Determination of low levels of sulfate (to approximately 20mg/L SO42-) by thermometric titration.

Standardization of 0.1mol/L perchloric acid in glacial acetic acid by catalyzed endpoint thermometric titration.

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

Determination of low levels of chloride (to approximately 5 mg/L Cl-) by thermometric titration.

This Application Note describes the determination of fluoride in silicon etch solutions with thermometric titration.

This Application Note explains how fluoride determination in acid etching baths can be performed with thermometric titration.

Standardization of 0.1 mol/L ammonium ferrous sulfate solution for use in thermometric titration of Cr(VI) solutions.

This Application Note outlines the determination of total acidic active surface sites in zeolites with thermometric titration.

This Application Note shows that the parameter of surface basicity of zeolites can be measured by thermometric titration.

This Application Note discusses the standardization of thiosulfate titrant for use in the determination of copper with thermometric titration.

Thermometric titration is presented as a simple, fast, and reliable method to determine calcium content in various drilling fluids.

Nitric acid, phosphoric acid, and acetic acid are easily determined in etching baths using thermometric titration (TET). Compared to potentiometric titration, TET is faster and more convenient. Analysis is complete in less than two minutes.

Thermometric titration quickly and accurately assesses the total solids content of fluids employed in drilling oil and gas wells within minutes.

This Application Note looks at the determination of ferrous ion in acidic solutions through redox titration with potassium permanganate as titrant and thermometric titration.

Determination of chlorite by direct thermometric titration with standard sodium thiosulfate solution. The procedurewas applied originally to the determination of chlorite in hide treatment solutions.

This Application Note describes the determination of the total sodium content in instant noodles which are also called «two minute noodles» in some countries. These products contain considerable amounts of sodium (at least 50% of the recommended daily dosage), which means that precise analysis of the sodium content is required. Argentometric titration of the chloride content (assuming that the sodium content in the noodles originates exclusively from the sodium chloride that is added to them) is unsuitable for precise analysis, as the nutrient contents listed on the product packaging document the presence of additional sodium salts other than sodium chloride. Thermometric titration enables fast and direct determination of sodium. 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

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.

This Application Note describes the determination of nitrite using thermometric endpoint titration with sulfamic acid. The nitrite content of a solution can be analyzed down to 0.2 mmol/L.

This Bulletin describes three potentiometric, one photometric, one thermometric and one conductometric titration method for sulfate determination. The question of which indication method is the most suitable depends primarily on the sample matrix.Method 1: Precipitation as barium sulfate and back titration of the Ba2+ surplus with EGTA. Use of the ion-selective calcium electrode as indicator electrode.Method 2: As with Method 1, although with the electrode combination tungsten/platinum.Method 3: Precipitation titration in semi-aqueous solution with lead nitrate in accordance with the European Pharmacopoeia using the ion-selective lead electrode as indicator electrode.Method 4: Photometric titration with lead nitrate, dithizone indicator and the Optrode 610 nm, particularly suitable for low concentrations (up to 5 mg SO42- in the sample solution).Method 5: Thermometric precipitation titration with Ba2+ in aqueous solution, particularly suitable for fertilizers.Method 6: Conductometric titration with barium acetate in accordance with DIN 53127

Silver and nitric acid are determined in silver electrolyte solutions by means of thermometric titration. The method provides accurate results in a short time and is ideally suited for routine process control.

Determination of Fe3+ and Cu2+ in copper refining solutions by thermometric titration. It was found that the conventional approach of masking Fe3+ to permit the iodometric determination of Cu2+ is not possible in some copper refining solutions.

A measured amount of salt is titrated directly with a solution of 1 mol/L tetrasodium EDTA to thermometrically determined endpoints for Ca and Mg. Acetylacetone is added to alter the Ca and Mg EDTA stability constants for better endpoint sharpness.

Sulfate is precipitated by reaction with an acidified barium chromate solution. The excess barium chromate is precipitated by basification with ammonia solution. Residual soluble chromate equivalent to the sulfate content of the sample is titrated with a solution of standard ferrous ion to a thermometrically determined endpoint.

Sulfate is precipitated as barium sulfate by reaction with an acidified barium chromate solution. The excess barium chromate is precipitated by basification with ammonia solution. Residual soluble chromate, equivalent to the sulfate content of the sample, is titrated with a solution of standard ferrous ion to a thermometrically determined endpoint.

Excessive silica concentrations in the boiler feed water can lead to deposits on turbine blades and must therefore be avoided. Silica analysis is carried out via differential photometry using a leading-edge technology thermostatic cuvette module for non-sample contact at the detector. Typical concentration ranges for silica are 0–50 ppb and 0–1 ppm or higher.

Determination of tar acids in coal tar products. This procedure may also be applied to the determination of a range of weakly acidic organic compounds such as carboxylic acids, hydroxy acids, phenols, phenolic acids, keto-enols, imides, and aromatic nitro compounds.11 Vaughan, G. A. Thermometric and Enthalpimetric Titrimetry. Van Nostrand Reinhold Co. Ltd (1973)

The presence of the hydrated ion [Fe(H2O)6]3+ can interfere with the determination of «free acid» due to the low pKa value (~2.2) of this ion. Ions of metals such as Fe, Cu, and Al can be masked effectively with fluoride, and permit the determination of the acid content by thermometric alkalimetric titration with good accuracy and precision.

A direct thermometric titration (TET) with 2 mol/L NaOH is used to determine the HF, NH4F, and maleic acid (C4H4O4) contents of acid cleaning solutions. Three endpoints (EPs) are obtained, which may be assigned as follows:EP1: C4H4O4 (pKa1 = 1.9), HF (pKa = 3.17)EP2: C4H4O4 (pKa2 = 6.07)EP2: NH4F (pKa = 8.2)The HF content is determined by subtracting the difference (EP2-EP1) from EP1.

Fertilizers are applied in the agricultural sector to provide more essential nutrients to growing plants. The so-called «NPK» fertilizers provide such nutrients to plants with its three main components (N – nitrogen, P – phosphorous, K – potassium). In fertilizers, nitrogen is mainly provided in three forms: as ammonium nitrate (NH4NO3), ammonia (NH3), and urea (H2NCONH2). Determination of the individual nitrogen-contributing components is often laborious work. Thermometric titration offers the possibility to rapidly determine the amount of ammoniacal nitrogen and urea nitrogen in a single titration using sodium hypochlorite as titrant.

A measured amount of milk is treated with trichloroacetic acid to coagulate milk solids and liberate calcium and magnesium as dissociated ion. The coagulated milk is filtered or centrifuged, and an aliquot of the clear serum is titrated with a standard solution of 1 mol/L tetra-sodium EDTA to thermometrically determined endpoints for Ca and Mg. Acetylacetone is added to alter the Ca- and Mg- EDTA stability constants for better endpoint sharpness.

Automated determination of total acid number (TAN) in new and used lubricating oils and crude oils using the 814 USB Sample Processor. Dissolve oil sample in mixture of toluene and 2-propanol, add paraformaldehyde and titrate with 0.1 mol/L or 0.01 mol/L KOH in propan-2-ol. The endpoint is indicated by an endothermic response caused by the base-catalyzed depolymerization of paraformaldehyde.Reference: 1. M. J. D. Carneiro, M. A. Feres Júnior, and O. E. S. Godinho. Determination of the acidity of oils using paraformaldehyde as a thermometric end-point indicator. J. Braz. Chem. Soc. 13 (5) 692-694 (2002)

Titration of an unfiltered suspension of the sample with a standardized solution of aluminum containing a stoichiometric excess of potassium ions in the presence of ammonium hydrogen difluoride at ~ pH 3 to give an exothermic reaction, forming insoluble NaK2AlF6. The titrant is standardized against a solution prepared from anhydrous sodium sulfate or sodium carbonate. 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

Potash is commonly mined from ore, deposited after ancient inland oceans evaporated. The potassium salt is then purified in evaporation ponds. At the end of this process, the potash is typically obtained as potassium chloride. Potash is mainly used as fertilizer, providing potassium—an essential nutrient—to plants. Additionally, it is used in the chemical industry and to produce medicine. Potassium content in potash is typically determined by flame photometry (F-AES) or ICP-OES. However, these techniques have high investment and running costs. By applying the historically used gravimetric precipitation reaction as a thermometric titration, it becomes possible to rapidly and inexpensively determine the potassium content in potash within minutes.

This Application Note describes the determination of the total concentration of sodium in precursor solutions used in the manufacturing of margarine. The solutions of the precursors are mixed with edible fats and oils to make margarine. Traces of sodium chloride and other sodium and potassium salts may be added to the margarine during this process, usually in the form of emulsifiers, stabilizers, antioxidants, vitamins, coloring agents or flavor enhancers. The analysis of the total sodium content in the precursor solutions is more efficient and cost-effective for the manufacturers than later total sodium content analyses in the final product.As a rule, argentometric titration of chloride is used for indirect determination of the sodium content of foodstuffs. The assumption behind this approach is that the chloride ions are present in a molar ratio of 1:1 with the sodium ions. This is however not the case when – as is usually the case with foodstuffs containing sodium – additional compounds containing sodium are also present in the margarine. The use of potassium chloride as a partial replacement for sodium chloride in some formulations is an additional source of error.The direct titration of sodium by means of thermometric endpoint titration (TET) eliminates these problems. TET is a direct determination method that not only takes into account the entire sodium content present in the solution but is also not hampered by the presence of potassium ions. 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

Metal-organic compounds are commonly used in organic chemistry, for example as Grignard reagents or as strong bases (e.g., butyl lithium compounds). The knowledge of the exact content of reactive species allows to better plan the required amounts for reactions preventing the waste of material or too low yields.This Application Note describes the analysis of metal organics by thermometric titration using 2-butanol as titrant. Due to the strongly exothermic nature of the reaction between 2-butanol with metal-organic compounds, a fast and quantitative analysis of these substances is possible.

Thermometric titration of nickel in electroless plating solution with disodium dimethylglyoximate.

Thermometric complexometric titration of metals is often performed with tetrasodium EDTA. This Application Note explains the standardization of tetrasodium EDTA titrant with copper.

Coagulation and flocculation are an essential part of treating both drinking water and wastewater. Aluminum salts such as aluminum sulfate and polyaluminum chloride (PAC) are often used for this purpose. For the precise application and exact dosage of the flocculant, it is important to accurately determine its aluminum content. In this Application Note, the aluminum content is accurately and reliably analyzed based on ABNT NBR 11176 using the 859 Titrotherm equipped with a Thermoprobe HF and sodium fluoride as titrant.

The determination of the acid number plays a significant role in the analysis of petroleum products. This is manifested in the numerous standard procedures in use over the world (internal specifications of multinational companies, national and international specifications of ASTM, DIN, IP, ISO, etc.). These procedures differ mainly in the composition of the used solvents and titrants.This bulletin describes the determination of the acid number in petroleum products by applying different types of titration.The potentiometric determination is described according to ASTM D664, the photometric according to ASTM D974 and the thermometric titration according to ASTM D8045.

As the determination of the exact content of individual glycerides in fats and oils is difficult and time-consuming, several fat sum parameters or fat indices are used for the characterization and quality control of fats and oils. Fats and oils are not only essential for cooking, they are also an important ingredient in pharmaceuticals and personal care products, such as ointments and creams. Consequently, several norms and standards describe the determination of the most important quality control parameters. This Application Bulletin describes eight important analytical methods for the following fat parameters in edible oils and fats:Determination of water content in accordance with the Karl Fischer method; Oxidation stability in accordance with the Rancimat method; Iodine value; Peroxide value; Saponification value; Acid value, free fatty acids (FFA); Hydroxyl number; Traces of nickel using polarography; Special care is taken to avoid chlorinated solvents in these methods. Also, as many of the mentioned methods as possible are automated.

Determination of Total Acid Number (TAN) values in biodiesel to <0.05 mg KOH/g sample.

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.

This Application Note explains how to use magnesium to standardize tetrasodium EDTA titrant.

The determination of the total base number (TBN) in motor oils is accomplished by means of titration with a standard solution made up of trifluoromethanesulfonic acid in glacial acetic acid and isobutyl vinyl ether as reagent for improved end point identification.

The bromine number indicates the degree of unsaturation and relies on the simple addition of bromine to the double bonds of alkenes. One mole of bromine is consumed for each mole of carbon-carbon double (C=C) bond present in a substance. In petroleum products, the bromine number corresponds to the olefin content.Normally, chlorinated solvents are used for the determination of the bromine number. In this Application Note they have been replaced by toluene. This makes the determination more ecological. The titration is performed automatically on an OMNIS system in combination with a double Pt-wire electrode. With this setup, a fast and accurate determination by potentiometric titration can be realized.

This Application Bulletin shows the determination of the total base number in petroleum products by applying different titration types according to various standards.

This Process Application Note details the simultaneous online analysis of H2S and NH3 in sour water which was previously treated in the sour water stripper (SWS). The method includes automatic cleaning and calibration. Fast and accurate results are continuously supplied for process control.

Online mercaptan and H₂S monitoring with the 2060 TI Ex Proof Analyzer certified for Zone-1 and Zone-2 areas.

This Process Application Note is dedicated to the online analysis of zinc, iron and sulfuric acid in several stages of the zinc production process. Additionally, traces of germanium, antimony, as well as several transition metals (e.g., Ni, Co, Cu, Cd) can be precisely determined (<50 µg/L) in the purification filtrates and reactor trains.

It is essential to know before starting the sample analysis if the electrode is in a good state or not. A well workingelectrode will increase the quality of your results, as the accuracy and precision will be increased. Furthermore, tedious error tracking can be omitted and no sample is wasted due to a defect or old electrode. There exist several ways how to check metal electrodes, e.g., measurement of redox potentials, potentiometric titration or bivoltammetric titration. This bulletin describes the best methods for the various by Metrohm available metal electrodes.

In addition to its natural occurrence in fruit and vegetables, ascorbic acid (Vitamin C) is used as an antioxidant in foods and drinks. Ascorbic acid is furthermore also to be found in numerous drugs.Ascorbic acid and its salts and esters can be determined with titration or by using polarography, for which ascorbic acid is oxidized to form dehydroascorbic acid.Bi-voltammetric or photometric equivalence point indication can be used for titrimetric determination. It must be taken into account here that only bi-voltammetric indication is independent of the inherent color of the sample. Polarography is the most selective of the methods described, as other reducing or oxidizing substances are not recorded.

Anionic surfactants can be titrated with cationic surfactants and vice-versa. The Bulletin describes a multitude of substances that can be determined in this fashion and specifies the respective working conditions and parameters. In contrast to the classic two-phase titration in accordance with Epton, the titration with the anionic and cationic surfactants electrodes can be performed without chloroform. Furthermore, the equivalence point of the titration is difficult to determine in some cases with the Epton method and the titration cannot be automated.In many cases, a surfactant ISE is a remedy that is both environmentally friendly and suitable here. It was developed specially for application with potentiometrically indicated surfactant determinations.

Pyrithione complexes, such as zinc pyrithione (ZnPT), copper pyrithione (CuPT), and sodium pyrithione (NaPT), are used as fungicides and bactericides. ZnPT is used in the treatment of skin conditions such as seborrheic dermatitis or dandruff. Furthermore, ZnPT is sometimes used as an antibacterial agent in paints to prevent algae and mildew growth. CuPT is primarily in use as a biocide to prevent biofouling of surfaces submerged in water. Meanwhile, NaPT is used as antifungal agent for treatment of mycosis, such as athlete’s foot. The different pyrithione complexes are determined by iodometric titration using a maintenance-free Pt Titrode for the indication.

In this application note, a fully automated system is presented which allows the determination of several parameters according to various standards within one analysis. These include conductivity (ISO 7888, EN 27888, ASTM D1125, EPA 120.1), the pH value (EN ISO 10523, ASTM D1293, EPA 150.1), alkalinity (EN ISO 9963, ASTM D1067, EPA 310.1), and Ca/Mg content (ISO 6059, ASTM D1126, EPA 130.2). Additionally, the system transfers the required sample volume into an external titration vessel for the analysis, reducing manual sample preparation. Furthermore, all sensors can be automatically calibrated and the titer of each titrant can also be determined.

In this application note, a fully automated system is presented which allows the determination of several parameters according to various standards within one analysis. These include conductivity (ISO 7888, EN 27888, ASTM D1125, EPA 120.1), pH value (EN ISO 10523, ASTM D1293, EPA 150.1), alkalinity (EN ISO 9963, ASTM D1067, EPA 310.1), and chloride content (ISO 9297, ASTM D512, EPA 325.3). Additionally the system transfers the required volume of sample into an external titration vessel, further reducing manual sample preparation. Furthermore, all sensors can be calibrated automatically and the titer of each titrant can also be determined.

In this application note, a fully automated system is presented which allows the determination of several parameters according to various standards within one analysis. These include conductivity (ISO 7888, EN 27888, ASTM D1125, EPA 120.1), pH value (EN ISO 10523, ASTM D1293, EPA 150.1), alkalinity (EN ISO 9963, ASTM D1067, EPA 310.1), Ca/Mg (ISO 6059, ASTM D1126, EPA 130.2), and chloride (ISO 9297, ASTM D512, EPA 325.3). Additionally the system transfers the required volume of sample into external titration vessels for the different analyses, reducing manual sample preparation. Furthermore, all sensors can be automatically calibrated and the titer of each titrant can also be determined.

Acid copper baths are mainly used for the copper deposition on semiconductor wafers. Small amounts of chloride increase the speed of deposition and reduce anode polarization. However, higher concentrations are undesired, as this will decrease the quality of the copper deposition. Therefore, it is quite important to monitor the amount of chloride to have an effective, yet high-quality copper deposition process.In this Application Note, a fully automated solution based on titration is presented. In comparison to ion chromatography, titration offers the benefit that no dilution of the sample is necessary, and the hardware is comparatively low-priced. Furthermore, the fully automated solution allows users to minimize handling errors, to reduce workloads, and to guarantee outstanding reproducibility.

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.

Lithium is a soft metal which is used for many applications, such as production of high-temperature lubricants or heat-resistant glass. Furthermore, lithium is used in large quantities in for battery production. It is obtained from brines and high-grade lithium ores. Depending on the lithium concentration, extraction may or may not be economically viable.This Application Note demonstrates a method to determine the lithium concentration in brines by potentiometric titration. Lithium and fluoride precipitate in ethanol as insoluble lithium fluoride. Using ammonium fluoride as the titrant and a fluoride ion-selective electrode (ISE), determination via potentiometric titration is possible. This method is more reliable, faster, and less expensive than the determination of lithium in brine by other more sophisticated techniques such as atomic absorption spectroscopy (AAS).

Corrosion of metallic components is an inherent problem for engines, because metals naturally tend to oxidize in the presence of water and/or low pH value. The reserve alkalinity of engine coolants and antirusts is a measure of the buffering ability to absorb acidity. The reserve alkalinity is frequently used for quality control during production and often listed in the specifications of the coolants. A fast and accurate determination is therefore important.This Application Note describes the straightforward determination of reserve alkalinity according to ASTM D1121. Using a fully automated system allows an accurate and reliable determination due to the reduction of human errors. Furthermore, the operator is free to carry out other tasks increasing the efficiency of the laboratory.

Sodium lactate is a salt form of lactic acid used in many regulated industries—therefore an accurate determination of the lactate content is required and is already covered in several norms. One such monograph by the US Pharmacopoeia (USP) results in high accuracies and well-defined titration curves but uses titrants and solvents that are more costly than necessary. In comparison, the presented modified method from Metrohm requires a 1:1 mixture of water and acetone and uses aqueous hydrochloric acid as titrant, resulting in an estimated cost reduction of 40% per titration compared to the USP method (USP–NF 2021, Issue 2). Furthermore, the time needed for each analysis is reduced to just 12% of the USP method (excluding blank determination). This Application Note presents both methods to determine lactate content and shows the results obtained on an OMNIS system.

Boric acid requires precise monitoring in the primary circuit to control nuclear reactor reactivity. The 2060 TI Process Analyzer monitors boric acid online in near-real time.

Reliable monitoring of TBC in styrene according to ASTM D4590 requires an explosion-proof solution like the 2060 TI Ex Proof Analyzer.

Precise online monitoring of peracetic acid (PPA) for beverage bottling requires a reliable stainless steel process analyzer.

In order to maintain product quality, the sodium chloride content in meat products must be monitored, as the limit values defined by the respective public health authorities must not be exceeded. The chloride content in food correlates with the salt content, its determination is therefore described in various norms and standards. However, preparation of meat samples is time consuming, as it requires homogenization with a mixer and a chloride extraction with water.In order to reduce workload and working hours, this Application Note describes a fully automatic potentiometric titration of chloride with silver nitrate in meat products based on ISO 1841-2, including fully automated sample preparation using a Polytron homogenizer.

ASTM D8192 describes the photometric titration of the total hardness, calcium hardness, and magnesium hardness in water with an optical sensor for objective endpoint indication, increasing precision and reliability. The method is suitable for both colored and colorless samples such as groundwater, surface water, wastewater, and drinking water. Using a fully automated OMNIS system equipped with an Optrode ensures that the sample preparation and analysis are repeatable.

Vitamin C, also known as ascorbic acid or L-ascorbic acid, is an essential nutrient involved in the repair of tissues and the enzymatic production of certain neurotransmitters. It is required for the functioning of several enzymes and immune performance, and is also an important antioxidant. This nutrient is found in many foods and is often used as a dietary supplement.This Application Note describes the photometric determination of ascorbic acid according to the standard ISO 6557-2. To increase the objectivity on the determined equivalence point and the reproducibility of the results, an autotitrator equipped with a photometric sensor, the Optrode, is used. The titrant 2,6-Dichlorophenol-indophenol (DCIP or DPIP) simultaneously serves as titrant and indicator.

The saponification value evaluates edible oil quality by indicating the average molecular weight of fatty acids. Its titrimetric determination in canola and olive oil is described here.

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.

The permanganate index (PMI) is a sum parameter that indicates the total load of oxidizable organic and inorganic matter in water. The substances concerned are mainly humic materials/acids that are primarily formed when dead organic material present in soil is further broken down and released into water sources. As it is an indicator of the water quality, testing of the PMI for drinking water is obligatory in many countries.For the determination, it is necessary to heat the stabilized water sample to 95 °C and higher for a stipulated time. Afterwards, the amount of permanganate that has remained after the reaction with the sample is determined titrimetrically. This sample preparation step requires considerable manual effort.In this Application Note, a fully automated procedure for the determination of the PMI according to GB/T 11892 is described, including all sample preparation steps. The gains in productivity because of a reduced manual workload are considerable.

Lithium salts (e.g., lithium carbonate and lithium hydroxide) are used in myriad applications. Lithium hydroxide is used for the production of lithium stearate, an important engine lubricant. In addition, it is utilized as an air purifier due to its ability to bind carbon dioxide. While the majority of lithium carbonate is used for aluminum production, it is also used for the glass and ceramic industry. It lowers the melting point of these materials, lowering the associated electricity costs and making it cheaper to produce them.For all of these applications, it is important to know the quality of the pure lithium salts used in the various production processes. This Application Note presents an easy method for the assay of lithium hydroxide and lithium carbonate on an automated OMNIS system.

Boehm titration is a quantitative analysis of functional groups on the surface of carbon materials based on their reactions with basic solutions of NaHCO3 (pKa = 6.4), Na2CO3 (pKa = 10.3), and NaOH (pKa = 15.7). This is a cost-efficient method that gives absolute values with high precision of the accessible, mainly oxygen-containing functional groups on the surface. Originally, Boehm titration was developed for carbon materials like conductive carbon black (CCB), activated carbon, porous carbon, and graphite. Modern carbon-based materials like graphene, graphene oxide (GO), or carbon nanotubes can also be analyzed this way.

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 standardization of the cationic surfactant TEGOtrant is performed using potentiometric titration as well as near-infrared spectroscopy (NIRS) in this application.

This white paper summarizes the advantages and benefits of automated titration in comparison to manual titration. The increase in accuracy and precision of measurements as well as significant time and cost savings are discussed.