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This Application Bulletin gives an overview of the volumetric water content determination according to Karl Fischer. Amongst others, it describes the handling of electrodes, samples, and water standards. The described procedures and parameters comply with the ASTM E203.

This Application Bulletin gives an overview of the coulometric water content determination according to Karl Fischer.Amongst others, it describes the handling of electrodes, samples, and water standards. The described procedures and parameters comply with the ASTM E1064.

The bromine number and bromine index are important quality control parameters for the determination of aliphatic C=Cdouble bonds in petroleum products. Both indices provide information on the content of substances that react withbromine. The difference between the two indices is that the bromine number indicates the consumption of bromine in gfor 100 g sample and the bromine index in mg for 100 g sample.This Application Bulletin describes the determination of the bromine number according to ASTM D1159, ISO 3839, BS2000-130, IP 130, GB/T 11135 and DIN-51774-1. The bromine index determination for aliphatic hydrocarbons is described according to ASTM D2710, IP 299, GB/T 11136 and DIN 51774-2. For aromatic hydrocarbons the determination of the bromine index is described according to ASTM D5776 and SH/T 1767. UOP 304 is not recommended for the determination of the bromine number or bromine index because its titration solvent contains mercuric chloride.

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.

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.

This bulletin describes a procedure to determine the bromine index (BI) using coulometric titration. The bromine index is the fraction of reactive unsaturated compounds (mostly C=C double bonds) in hydrocarbons encountered in the petrochemical industry. The double bonds are split with the attachment addition of bromine.

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.

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

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.

Determination of Total Acid Number (TAN) values in mineral oils and similar 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.

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.

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.

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.

This Application Note describes the determination of the water content in transformer oil using the oven technique.

The bromine index indicates the degree of unsaturation and relies on the simple addition of bromine to the double bond of alkenes. One mole of bromine is consumed for each mol of carbon-carbon double bond. The bromine index indicates the olefin content in aromatic hydrocarbons. This Application Note describes the determination by coulometric titration according to ASTM D1492.

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.

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 chloride, nitrite, nitrate, phosphate, and sulfate in cutting oil emulsion using anion chromatography with conductivity detection after chemical suppression and dialysis for sample preparation.

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

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 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.

Basic additives are added to petroleum products to inhibit corrosion as they have a neutralizing effect on acidic compounds, which are formed as a result of degradation processes. Total base number (TBN) indicates the amount of basic additives present and thus can be used as a measure for the degradation of the petroleum product.Using an automated titration system with a photometric sensor to detect the end point ensures that the titrations are always carried out under the same conditions. This improves the precision and reliability of the results.This Application Notes describes the fully automated photometric determination of TBN in used engine oil using the Metrohm Optrode for the indication of the methyl orange endpoint (at 520 nm).

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.

For titrations in low conducting media (e.g., non-aqueous titrations) the potentiometric indication can be disturbed by interfering signals. When differential amplification is used, these signals are measured by both the measuring electrode and the reference electrode and thus neutralized. It is therefore possible to obtain smoother titration curves and more reproducible results.This Application Note describes the potentiometric determination of the acid number and base number in used motor oil by the differential amplification using a fully automated OMNIS system.

The bromine number is an important parameter for the determination of aliphatic C=C double bonds in petroleum products. The bromine number is usually determined using electrochemical titration at 5 °C, where the bromine is generated in situ from a bromide/bromate solution. For the titration, a solvent mixture of glacial acetic acid, methanol, and chloroform is used. In this Application Note, the toxic chloroform was replaced with diethyl carbonate.

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.

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 bromine index is an important parameter for the determination of aliphatic C=C double bonds in petroleum hydrocarbons. For the titration, a solvent mixture of glacial acetic acid, methanol, and dichloromethane is usually used.In this Application Note, the chlorinated solvent in the solvent mixture was replaced with toluene, resulting in a more environmentally beneficial method in comparison to ASTM D2710 and IP 299.

The bromine index is an important quality control parameter for the determination of aliphatic C=C double bonds in aromatic hydrocarbons and is thus a measure for the presence of aliphatic unsaturation in these materials. In situ generated bromine reacts with the aliphatic double bonds. When the titration is finished an excess of free bromine causes a sudden change in the measured potential thus indicating the equivalence point.

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.

Near-Infrared spectroscopy (NIRS) is a widely used analytical technique for quantitative analysis of various products in research and industrial applications. This white paper summarizes the workflow of the development of quantitative methods according to ASTM E1655.

Quality control is impacted by multiple challenges, which can have an influence on the functioning of the QC lab. The present White Paper provides approaches, how to simplify the daily quality control using near-infrared spectroscopy combined with a dedicated smart software like Vision Air.

The acid number (AN) is a measure for the quality of oils and their potential to enhance corrosion. When analyzing fresh, unused oils, the AN is used to ensure the specified quality from the manufacturer, whereas for used oils the AN is determined to observe its increase until a critical level is reached. Although it is generally assumed that the AN correlates to the corrosive potential of the oil, this is not exactly correct, as it is the change of the AN value which indicates this issue. Therefore it is necessary to determine the AN on a regular basis.Several standards already exist to determine AN via titration methods, however it is also possible to measure this parameter via spectroscopic (NIRS) methodology. No matter which technique you choose, Metrohm has you covered with high-performance instruments suitable for these published norms.

Underestimation of quality control (QC) processes is one of the major factors leading to internal and external product failure, which have been reported to cause a loss of turnover between 10–30%. As a result, many different norms are put in place to support manufacturers with their QC process. However, time to result and the associated costs for chemicals can be quite excessive, leading many companies to implement near-infrared spectroscopy (NIRS) in their QC process. This paper illustrates the potential of NIRS and displays cost saving potentials up to 90%.

Knowledge of the water content in lubricating oils, additives, and similar products is important in the manufacturing, purchase, sale, or transfer of petroleum products to help estimate their quality and performance characteristics. Monitoring the water content in such products can prevent damage to infrastructure and ensure safe operation by avoiding corrosion processes and subsequent engine wear. This White Paper explains the easy determination of moisture in petroleum samples by coulometric Karl Fischer titration according to the three procedures outlined in ASTM Method D6304. A comparison is given between the procedures to determine which is most suitable for different sample types.

Voltammetry (VA) is a fast and established method for testing the remaining antioxidant content in industrial lubricants. The flexible and modular Metrohm VA system setup discussed in this White Paper delivers more repeatable and more reproducible results which fulfill all ASTM requirements. Additionally, users can automate the complete analysis process which makes it possible to run series of samples completely unattended.

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