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Only coulometric Karl Fischer titration can determine low water contents with sufficient accuracy.This Application Bulletin describes the direct determination according to ASTM D6304, ASTM E1064, ASTM D1533, ASTM D3401, ASTM D4928, EN IEC 60814, EN ISO 12937, ISO 10337, DIN 51777, and GB/T 11146. The oven technique is described according to ASTM D6304, EN IEC 60814, and DIN 51777.

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

This Application Bulletin contains installation instructions for the MVA-25 (with automatic sample preparation) used to measure antioxidants in lubricants.

Determination of zinc, sodium, calcium, and magnesium in an industrial bath containing cooling lubricants using cation chromatography with direct conductivity 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.

Isopropylamine and dicyclohexylamine are used as emulsifiers and need to be determined in emulsions along with standard cations. However, emulsions must not be injected directly into the ion chromatograph as the organic components may damage the ion exchanger stationary phase in the separation column. Inline Dialysis as sample preparation is the perfect tool for such samples. The ions of interest are separated from the organic phase by diffusion through the hydrophilic membrane, thus protecting the column. Full automation makes the analyses even easier and more efficient for the user.

Paraffin and lubricating oils are yielded from the wax fraction of raw oil distillation. The chloride content of both should be low. This Application Note describes chloride determination after inline combustion. Although it does not happen in this application, this method can also be used to quantify the sulfur content.Keyword: pyrohydrolysis

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

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

Determination of chloride in oil well drilling fluids.

Determination of moisture in lubricating oils with TEOF (triethyl orthoformate).

Determination of water in automotive lubricating oils.

Determination of low content of HCl (around 10 ppm) in silicone oil.

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)

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.

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

The water content of turbine oil is determined according to Karl Fischer. Because of the low water content of the sample, coulometric titration is used.

The water content of used lubricating oil is determined according to Karl Fischer by coulometric titration. To prevent unwanted side reactions special KF reagents are used.

The water content of silicone oil is determined according to Karl Fischer by coulometric titration.

Moisture in petroleum products causes several issues: corrosion and wear in pipelines and storage tanks, an increase in debris load resulting in diminished lubrication, blocked filters, or even harmful bacterial growth. As a result, increased water content can lead to infrastructure damage, higher maintenance costs, or even unwanted downtimes.Coulometric Karl Fischer titration is the method of choice for low water content in petroleum products. Using a Karl Fischer oven to vaporize the water present in the sample prior to titration not only greatly reduces matrix interferences, it can also be fully automated. This allows a reliable and cost-efficient analysis of the water content according to ASTM D6304 (Procedure B) in products such as diesel, hydraulic oil, lubricant, additive, turbine oil, and base oil.

For lubricant analysis, determination of the Acid Number (ASTM D664), viscosity (ASTM D445), moisture content (ASTM D6304), and color number (ASTM D1500) require the use of multiple analytical technologies and, in part, large volumes of chemicals. This application note demonstrates that the XDS RapidLiquid Analyzer operating in the visible and near-infrared spectral region (Vis-NIR) provides a fast and cost-efficient alternative for the determination of the AN, viscosity, moisture content, and color number of lubricants. With no sample preparation or chemicals needed, Vis-NIR spectroscopy allows for multi parameter analysis of lubricants in less than one minute.

This Application Note demonstrates the data transfer from a Fourier transform to a dispersive NIR instrument, using quality control of lubricating oils as an example application. It is shown that FT-NIR instruments can be replaced by dispersive ones without time-consuming sample remeasurement and subsequent method development.

Acid Number (AN) analysis of lubricants (ASTM D664) can be a lengthy and costly process due to usage of large amounts of chemicals and required cleaning steps of the analytical equipment between each measurement. This application note demonstrates that the XDS RapidLiquid Analyzer operating in the visible and near-infrared spectral region (Vis-NIR) provides a cost-efficient, fast alternative for the determination of the acid number of lubricants. With no sample preparation or chemicals needed, Vis-NIR spectroscopy allows for the analysis of AN in less than a minute.

Alkaline additives in engine lubricants are used to prevent the build-up of acids and as a result, they inhibit corrosion. The total base number (TBN) indicates the amount of basic additives present in samples and thus can be used as a measure for the degradation of the lubricant. The standard test method for TBN in lubricants is potentiometric titration according to ASTM D2896. This method requires the use of toxic reagents involves a labor-intensive cleaning procedure. In contrast to the primary method, near-infrared spectroscopy (NIRS) is a fast analytical technique which does not produce any chemical waste and completes the TBN analysis in less than one minute.

Glycol solutions act as antifreeze agents and are often used as such in motor vehicles. Due to the toxicity of (mono)ethylene glycol (MEG), use is being increasingly expanded to the non-toxic propylene glycol. This Application Note presents the separation and quantification of the two glycols. Separation is performed on the Metrosep Carb 2 - 250/4.0 column. Due to the absence of chromophores and the low conductivity of the glycols, pulsed amperometric detection (PAD) is used to facilitate determination.Key words: ethanediol, propanediol

A safer way to monitor moisture content in crude distillation unit overhead fractions is with inline near-infrared spectroscopy using the 2060 The NIR-Ex Analyzer.

The oxidation stability of biodegradable lubricating oil is determined using the Rancimat method.

Motor oils are exposed to high shear forces and temperatures while the motor is running. Mechanical abrasions set iron and copper free, which act as catalysts for oxidation. All of this decreases the durability of motor oils. The oxidation stability with iron and copper catalysts can give an approximate indication for the shelf life. A reproducible and accurate determination of the oxidation stability using the 892 Professional Rancimat can be realized.

Determination of sulfate in diesel engine coolant using anion chromatography with conductivity detection after chemical suppression and dialysis for sample preparation.

Determination of traces of chloride in a technical product using anion chromatography with conductivity detection after chemical suppression.

Determination of chloride, nitrite, nitrate, and sulfate in cooling lubricants using anion chromatography with conductivity and UV detection (230 nm) after chemical suppression and inline sample preparation by dialysis.

Determination of chloride, nitrite, and sulfate in a used zinc bath using anion chromatography with conductivity detection after chemical suppression.

Determination of fluoride, acetate, formate, and chloride in a brake fluid using anion chromatography with conductivity detection after chemical suppression.

Determination of glycolate, formate, chloride, nitrite, nitrate, phosphate, sulfate, and oxalate in engine coolant using anion chromatography with conductivity detection after chemical suppression.

Determination of chloride, nitrite, bromide, nitrate, phosphate, sulfite, sulfate, and oxalate in a cooling lubricant using anion chromatography with conductivity detection and subsequent UV detection (see AN-U-047) after sequential suppression and Metrohm Inline Dialysis.

Determination of fluoride, formate, chloride, nitrite, bromide, nitrate, sulfate, oxalate, and molybdate in a coolant using anion chromatography with conductivity detection after chemical suppression and Metrohm Inline Dialysis.

This Application Note describes the determination of total content of Ba, Ca, Mg, Pb and Zn in unused lubricating oil by means of the Optrode (610 nm). An excess of EDTA is first added to the metals. Afterwards, the excess EDTA is titrated back with magnesium chloride solution up to the end point of the indicator Eriochrome Black T.

The acid number (AN) of insulating, transformer, and turbine oils is crucial to ensure safe operation, operating equipment control, and corrosion prevention. These oils generally have low AN specifications and their AN determination by manual color-indicator titration is difficult, especially when analyzing colored samples.Using a Titrator with a photometric sensor to detect the end point ensures that the titrations are always carried out under the same conditions. This greatly increases the precision and reliability of the results, which in turn results in improved monitoring for your operations.

Fresh as well as used petroleum products may contain acidic components as additives or degradation products. The acid number (AN) is a measure for the relative amount of acids present expressed as mg KOH per g sample. Moreover, AN is used as a quality parameter of lubricating oils both for assessing the quality of new formulations and as an indicator for the degradation of such formulations during service. The use of a pH electrode suitable for non-aqueous titrations ensures the reliable determination of the equivalence point. A flexible sleeve diaphragm facilitates its cleaning especially after use in heavily contaminated samples, such as in used engine oils. Using the correct electrode greatly increases the precision and reliability of the results. This Application Note describes the potentiometric determination of the acid number according to ASTM D664 and IP 177 using the pH electrode Solvotrode easyClean.

Basic chemicals are added to petroleum products to prevent corrosion as they neutralize acidic components that form during the use and aging of these products. The base number (BN) gives an indication regarding the amount of these basic additives present, and it can be used as a measure for the degradation of the petroleum product.This Application Note describes the potentiometric determination of the base number according to ISO 3771, ASTM D2896, and IP 276 using the Metrohm Solvotrode easyClean and a fully automated OMNIS system.

This Application Note describes the conductometric determination of the total base number in engine oil according to IP 400.

Fully automated determination of the total acid number and total base number in engine oils according to ASTM D664 and ASTM D2896 is possible with the OMNIS Titrator.

Corrosion of metallic components is an inherent problem for engines, because metals naturally tend to oxidize in the presence of water and/or acids. Increased acid content is indicated by a low pH value, and could lead to a variety of problems like a shorter storage life (stability) or a reduced buffer capacity of the used engine coolant or antirust.In this Application Note, engine coolants or antirust samples are dissolved in water, and the pH measurement using the Profitrode is carried out according to ASTM D1287.

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.

The total acid number (TAN) is an important parameter for assessing the acidity of oils and fuels. This Application Note determines TAN using conductometric titration.

Determination of nitrite and nitrate in a cooling lubricant using anion chromatography with conductivity detection (see AN S-274) and subsequent UV detection after sequential suppression and Metrohm Inline Dialysis.

Scale formation is a critical issue in cooling systems leading to system damage, which generates enormous operational losses. One important component of scale forming is silica. Amorphous silica and metal silicates especially tend to build up scale. Therefore, it is crucial to know the silica concentration in cooling agents. By ion chromatography with UV/VIS detection and PCR, it is possible to determine both free and total silicate content. Sample dilution in ultrapure water and direct injection delivers the free silicate concentration. The total silicate content is determined after hydrolysis of amorphous silica by sample dilution in alkaline eluent, and injection after a reaction time (e.g. 4 hours) prior to the analysis.

Formaldehyde is determined polarographically at the DME in alkaline solution.

Testing of in-service lubricating oils for their remaining antioxidant content is critical for capital equipment uptime as well as reducing running costs and repair expenses. Test methodologies such as RPVOT (rotating pressure vessel oxidation test) are time consuming and expensive to perform. Remaining Useful Life is a proven voltammetric method for testing the remaining active antioxidant content in minutes. Depending on the electrolyte, aromatic amine and phenolic antioxidants or hindered phenolic antioxidants can be determined.For the first time, a fully automated system is demonstrated, showing dramatically improved repeatability of data for confidence in reporting. Operator time is saved during sample preparation and irreproducible manual interpretation is eliminated via completely autonomous software processing. The user adds the sample into the vials, then the determination process of the sample series (including sample preparation and result calculations) is carried out automatically. The system is based on methods ASTM D6810, ASTM D6971, ASTM D7527, and ASTM D7590.

Improve petrochemical quality control with NIRS. Fast, cost-effective, and no sample prep needed. Learn more in our eBook.