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For the first time, glyphosate determination and that of its primary metabolite AMPA in drinking water using IC with pulsed amperometric detection (flexIPAD) in the low µg/L range are shown. Compared to HPLC analysis with a mass-selective detector, it is a very cost-effective method for determining the glyphosate and AMPA content in water and foodstuffs. With a detection limit at approx. 1 µg/L, compliance with limit values for glyphosate can be monitored in the USA, Canada, and Australia, among others.

The Rancimat method is a widely accepted method for the determination of the oxidation stability of natural fats and oils. Its main application is quality control in oil mills and the oil processing industry. At elevated temperatures and under the exposure of air, fatty acids are oxidized. The reaction products are absorbed in ultrapure water that is continually monitored for conductivity. After an induction period with slow reaction, the formation of volatile carboxylic acids is accelerated. At that time the conductivity begins to increase rapidly. Instead of investing weeks or months, the sample can be oxidized within a few hours.The method can also be used to determine the oxidation stability of solid foodstuffs that contain natural fats or oils. Frequently, a direct determination without extraction of the fat is possible, if the fat content exceeds a minimum level. In these cases, a simple and reliable assessment of the quality of the produced foodstuff is possible.A number of fat-containing solid foodstuffs such as almonds, peanuts, peanut-flavored puffs, potato chips, muffins, butter cookies, French fries, and instant noodles were successfully tested with the Rancimat method. The experiments revealed that the comminution of the sample is one of the most important steps. The grinding procedure of the tested samples was kept as simple as possible to avoid the use of expensive milling instrumentation.

Fructose (fruit sugar) is the only ketose that occurs naturally. It is found free in a mixture with dextrose (honey, sweet fruits, tomatoes) or bound as a component of cane sugar and various starch-like carbohydrates. As fructose tastes sweeter than dextrose, it finds great use as a sweetening agent.In 1932, the polarographic reducibility of sugar was described for the first time by Heyrovsky and Smoler. The following method can be used to determine the fructose content of fruit, fruit juice and honey quantitatively.

In the past, selenium determinations have always been either unreliable or have required complicated methods. However, as selenium is on the one hand an essential trace element (vegetable and animal tissues contain about 10 μg/kg), while on the other hand it is very toxic (threshold value 0.1 mg/m3), it is very important to cover determinations in the micro range. Cathodic stripping voltammetry (CSV) enables selenium to be determined in mass concentrations down to ρ(Se(IV)) = 0.3 μg/L.

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.

In most electrolytes the peak potentials of lead and tin are so close together, that a voltammetric determination is impossible. Difficulties occur especially if one of the metals is present in excess.Method 1 describes the determination of Pb and Sn. Anodic stripping voltammetry (ASV) is used under addition of cetyltrimethylammonium bromide. This method is used when:• one is mainly interested in Pb• Pb is in excess• Sn/Pb ratio is not higher than 200:1According to method 1, Sn and Pb can be determined simultaneously if the difference in the concentrations is not too high and Cd is absent.Method 2 is applied when traces of Sn and Pb are found or interfering TI and/or Cd ions are present. This method also uses DPASV in an oxalate buffer with methylene blue addition.

The Rancimat method determines the oxidation stability (OSI) and antioxidant capacity (SI) of solid foods. OSI measurements are performed directly, with extracted isolated fat, or via the polyethylene glycol method. SI can be determined when the sample is mixed with a reference of antioxidant-free fat.

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

Determination of free fatty acids (FFA) in oils.

NIRS enables rapid, chemical-free analysis of glucose, fructose, sucrose, and Brix in fruit juices without sample prep, offering a fast alternative to traditional methods.

Monitoring the iodine value in edible oil blends is crucial to produce vegetable oils with the desired properties. This Application Note displays the benefit of using the Metrohm NIRS DS2500 Liquid Analyzer for quality control in food laboratories.

Excess sodium intake increases the risk of health issues. Ion-selective electrodes (ISEs) offer a fast, accurate, and cost-effective method for measuring sodium in food.

The water content of flour is determined according to Karl Fischer. To shorten the analysis times and to obtain more precise results, the determinations are carried out at 50 °C.

Separation of polysaccharides with increasing numbers of inulin units using gradient elution and pulsed amperometric detection.

Maltodextrin is a polysaccharide consisting of glucose units. Maltodextrins are classified as dextrose equivalents (DE, with DE = 3–20). This application shows the determination of glucose (DE = 1), maltose (DE = 2) till maltoheptaose (DE = 7). The separation is achieved on a Metrosep Carb 2 - 250/4.0 column with subsequent pulsed amperometric detection (PAD).

Oxidation stability is an important parameter defining the quality of tea. It also provides information about the long-term stability of the naturally included antioxidants and thus the stability of the product. However, tea cannot be measured directly with the Rancimat method, as no evaluable induction time is obtained. The reason for this is that no measurable oxidation product is formed. However, using polyethylene glycol (PEG) as carrier material, many of these samples can be directly and reproducibly measured without any sample preparation. This is due to the antioxidants that are naturally present in the sample matrix, which stabilize the induction time of the PEG. The induction time can therefore be directly related to the oxidation stability of the sample.A reproducible and accurate determination of the oxidation stability is feasible using the 892 Professional Rancimat. In this Application Notes the oxidation stability of different teas is determined in this way. More information on the Rancimat method can be found on the Metrohm website.

Processing degrades antioxidant levels in spices. The 892 Professional Rancimat determines oxidation stability with the PEG method as per AOCS Cd 12b-92 and ISO 6886.

Determination of sulfite in ginger powder using anion chromatography with conductivity detection after chemical suppression and dialysis for sample preparation.

Determination of chloride in canned vegetables by potentiometric titration with silver nitrate using the Ag-Titrode.

In order to consistently manufacture high quality baked goods, it is critical to measure the pH value and acidity content in the raw materials and during the production steps. These factors have a major influence on the taste and storage lifetime of the final product. Consistent product quality is only possible with precise measurements during the process.This Application Note describes the measurement of pH value and the total titratable acidity in flour, dough, and bread using the Eco Titrator from Metrohm.

The iodometric back titration is a precise method used to accurately measure the caffeine content in various aqueous samples. Reliable determinations are made easy using the OMNIS Titrator equipped with a dPt Titrode.

The water content of lemongrass oil is determined according to Karl Fischer. To prevent unwanted side reactions, special KF reagents for aldehydes and ketones are used and the determination is carried out at 0 ... 4 °C.

Adulteration in the food industry is a significant concern due to potential health risks and changes in product quality and nutrition. Detecting such adulteration is challenging, however, to ensure high-quality products, precise measurements during the manufacturing process are essential for identifying any contamination in raw materials and final products. This Process Application Note details the inline analysis of potato starch in the wheat flour manufacturing process with a 2060 The NIR Analyzer from Metrohm Process Analytics.

This Application Note presents a modified time-saving method to determine iodine value (IV) in edible oils based on several standards (EN ISO 3961, ASTM D5554, etc.).

This Application Note describes the titration of acid value and free fatty acids in different edible oils, based on the standards EN ISO 660, USP<401>, and Ph.Eur. 2.5.1.

Traditional Chinese medicine (TCM) remedies are gaining popularity in other cultures. In some TCM, sulfur dioxide (SO2) is used as a preservative, antioxidant, and disinfectant. The products are treated by sulfurization with SO2 gas. However, sulfur dioxide is a very poisonous gas. Global health authorities have set strict limits for the content of SO2 in products. It is therefore of crucial importance to determine the sulfur dioxide content to comply with these limits. In this well-suited method, the SO2 content in different natural TCM products are analyzed reliably and accurately according to ISO 22590 using the Eco Titrator equipped with an Optrode and sodium hydroxide as titrant.

Efficiently analyze food products with ion chromatography (IC). Discover its robust applications in quality control for beverages, food additives, and dairy.

This study presents the automatic titration of low sulfite levels in beet crystal sugar using an OMNIS Titrator and a Pt Titrode as the potentiometric sensor.

Ion measurement can be conducted in several different ways, e.g., ion chromatography (IC), inductively coupled plasma optical emission spectrometry (ICP-OES), or atom absorption spectroscopy (AAS). Each of these are well-established, widely used methods in analytical laboratories. However, the initial costs are relatively high. In contrast, ion measurement by the use of an ion-selective electrode (ISE) is a promising alternative to these costly techniques. This White Paper explains the challenges which may be encountered when applying standard addition or direct measurement, and how to overcome them in order for analysts to gain more confidence with this type of analysis.

Sulfites are well-known additives in foods and beverages used to extend shelf life and preserve colors. Such properties have led to the broad usage of sulfites in a range of foodstuffs like fruits, cereals, vegetables, seafood, juices, alcoholic and non-alcoholic (soft) beverages, and in some meat products. The term «sulfites» describes a group of molecules that include sulfur dioxide (SO2) and chemically related molecules like sodium sulfite (Na2SO3), sodium bisulfite (NaHSO3), or sodium metabisulfite (Na2S2O5). Sulfite intake has been correlated with several adverse reactions, and therefore sulfites are included in the FAO/WHO Codex Alimentarius list. Labelling sulfite content in foods and beverages is necessary when the total concentration exceeds 10 mg/kg. Metrohm ion chromatography allows the reliable measurement of sulfite in different matrices using either conductivity or amperometric detection. The inclusion of automated sample preparation and cleaning steps with Metrohm instrumentation saves additional analyst time and helps increase sample throughput.

Potentiometric titration is an accurate method for determining chloride content. For detailed instructions and troubleshooting tips, download our Application Bulletin.

This Application Bulletin describes the voltammetric determination of the elements antimony, bismuth, and copper. The limit of detection for the three elements is 0.5 ... 1 µg/L.

This Bulletin describes analysis methods for determining the following parameters: pH value, total titratable acid, ash alkalinity, formol number, total sulfurous acid, chloride, sulfate, calcium, and magnesium. These methods are suitable for the analysis of jams, fruit and vegetable juices, and their concentrates.

This Application Bulletin describes the determination of mercury by anodic stripping voltammetry (ASV) at the rotating gold electrode. With a deposition time of 90 s, the calibration curve is linear from 0.4 to 15 μg/L; the limit of quantification is 0.4 μg/L.The method has primarily been drawn up for investigating water samples. After appropriate digestion, the determination of mercury is possible even in samples with a high load of organic substances (wastewater, food and semi-luxuries, biological fluids, pharmaceuticals).

Cadmium, lead, and copper can be determined simultaneously in oxalate buffer by anodic stripping voltammetry (ASV) after digestion with sulfuric acid and hydrogen peroxide. Tin present in the sample does not interfere with the determination of lead.For the voltammetric determination of tin please refer to Application Bulletin no. 176.

This Application Bulletin describes methods for the polarographic and voltammetric determination of small quantities of chromium in water, effluent water and biological samples. Methods for the sample preparation for various matrices are given.

Bromide is removed from the sample as BrCN by distillation. The BrCN is absorbed in sodium hydroxide solution and decomposed with concentrated sulfuric acid, then the released bromide ions are determined by potentiometric titration with silver nitrate solution. Iodide does not interfere with the determination.Iodide is oxidized to iodate by hypobromite. After destruction of the excess hypobromite, the potentiometric titration (of the iodine released from iodate) is carried out with sodium thiosulfate solution. Bromide does not interfere, even in great excess.The described methods allow the determination of bromide and iodide in the presence of a large excess of chloride (e.g., in brine, seawater, sodium chloride, etc.).

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.

Formaldehyde can be determined reductively at the DME. Depending on the sample composition it may be possible to determine the formaldehyde directly in the sample. If interferences occur then sample preparation may be necessary, e.g. absorption, extraction, or distillation.Two methods are described. In the first method formaldehyde is reduced directly in alkaline solution. Higher concentrations of alkaline or alkaline earth metals interfere. In such cases the second method can be applied. Formaldehyde is derivatized with hydrazine forming the hydrazone, which can be measured polarographically in acidic solution.

Cu2+, Co2+, Ni2+, Zn2+, and Fe2+/Fe3+ are determined simultaneously. Interference due to the presence of other metals is mentioned, and methods given to eliminate it. The threshold of determination is ρ = 20 µg/L for Co and Ni, and ρ = 50 µg/L each for Cu, Zn, and Fe.

It has been known for years that consuming too much nitrates from foodstuffs can result in cyanosis, particularly for small children and susceptible adults. According to the WHO standard, the hazard level lies at a mass concentration c(NO3-) ≥ 50 mg/L. However, more recent studies have shown that when nitrate concentrations in the human body are too high, they can (via nitrite) result in the formation of carcinogenic and even more hazardous nitrosamines.Known photometric methods for the determination of the nitrate anion are time-consuming and prone to a wide range of interferences. With nitrate analysis continually increasing in importance, the demand for a selective, rapid, and relatively accurate method has also increased. Such a method is described in this Application Bulletin. The Appendix contains a cselection of application examples where nitrate concentrations have been determined in water samples, soil extracts, fertilizers, vegetables, and beverages.

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

This application note describes the determination of the total sodium content in soy milk products. The methodology may also be applied to the determination of sodium in milk products from cows, goats and sheep. A standard addition technique is employed to permit the accurate and precise determination of sodium at relatively low levels.

Near-infrared spectroscopy (NIRS) is a fast, chemical-free analytical method for the simultaneous analysis of density, water activity, and moisture of green coffee beans.

Near-infrared spectroscopy (NIRS) is a fast, chemical-free alternative analytical technology for caffeine and moisture analysis in roasted coffee beans and grounds.

Near-infrared spectroscopy can quickly determine multiple edible oil quality parameters simultaneously without sample preparation as shown in this Application Note.

Near-infrared spectroscopy (NIRS) offers a fast, solvent-free alternative to traditional methods for assessing olive oil quality and detecting potential food fraud.

NIR spectroscopy offers fast, chemical-free analysis of ash, protein, moisture, and rheological properties in flour – ideal for routine lab or atline quality control.

This Application Note shows how NIR spectroscopy is used to determine the water content (moisture content), protein content, and fat content in whole and ground almonds.

NIR spectroscopy is an alternative method for olive pomace fat analysis. Unlike other conventional methods, NIRS requires no sample preparation nor chemical solvents.