Applications

The TacticID®-GP Plus has multiple measurement modes to support safety and security users. A-Mode allows the user to create library Raman or SERS spectra customizable for spectral search range and hit quality index (HQI) threshold. A-mode is of beneficial use to forensics laboratories that would like to utilize expansion of SERS detection of designer drugs specific to their geographical regions or for food safety in perspective markets. In this example, A-Mode is used to create a SERS library of melamine to easily detect the presence of melamine in infant formula using a single indicator peak.

The analytical challenge treated in the present work consists in the determination of chloride, phosphate and sulfate in the presence of difficult sample matrices that interact with the stationary column phase or even render it unusable. Metrohm`s patented stopped-flow dialysis coupled to the new 881 Compact IC pro ion chromatograph overcomes these drawbacks. Two standard solutions covering the concentration ranges 1.0…3.6 mg/L and 10…36 mg/L as well as two samples, an ultra-high temperature (UHT) processed milk and a baby milk powder, were characterized in terms of analyte concentration, relative standard deviation, calibration quality, carryover and recovery rates. While the five-point calibration curves yielded correlation coefficients (R) better than 0.9999, carryover (between two subsequent injections of a concentrated sample and a blank) was less than 0.49%. Recoveries for the low (10…36 mg/L) and high standard concentrations (1.0…3.6 mg/L) were within 91…99% and 94…100%, respectively. Automated compact stopped-flow dialysis is a leading-edge sample preparation technique that ensures optimum separation performance by effectively protecting the column from detrimental matrix compounds.

The analysis described in this poster dicusses thermometric titration as a promising method for the straightforward sodium determination in foodstuffs. Thermometric sodium titration was tested for its applicability to various food matrices such as soups, gravy and several salty snacks. Enthalpy change can be monitored as a change in temperature of the solution using a sensitive digital thermometer. The sodium determination described here relies on the exothermic precipitation of elpasolite (NaK2AlF6). The titrant is a standard aluminum solution which contains an excess of potassium ions. The titration is performed directly on a suspension of the food sample and is completed in under two minutes. The method is robust, can be fully automated and due to the highly reproducible high-frequency homogenization, copes with a variety of challenging food matrices (ketchup, instant soups, pretzels, etc.). 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

The potentiometric titration of Kjeldahl nitrogen is one of the most common analytic procedures. It is referenced in numerous standards, ranging from the food and animal feed industries through sewage and waste analysis and all the way to the fertilizer industry. As a rule, the samples are digested with concentrated sulfuric acid with the addition of a catalyst. The ammonium sulfate that is formed is distilled as ammonia in alkali solution, collected in an absorption solution and titrated there.This Bulletin provides a detailed description of potentiometric nitrogen determination following distillation of the digestion solution, followed by a discussion of the possibilities of coulometric titration (without distillation).

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.

The determination of sodium with the sodium ISE represents a selective, rapid, accurate, and favorably-priced method which is described in this Bulletin. Examples are used to show how determinations can be carried out with the 692 pH/Ion Meter using either direct measurement or the standard addition technique. The sodium concentration has been determined in standard solutions, water samples (tap water, mineral water, wastewater), foodstuffs (spinach, baby food), and urine. The construction, working principles, and areas of application of the two Metrohm ion-selective sodium electrodes – the 6.0501.100 Glass membrane ISE and the 6.0508.100 Polymer membrane ISE – are explained in detail.

This Bulletin describes methods for measuring the pH value of dairy products. Particular attention has been paid to the handling, maintenance, and storage of the pH electrodes.

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.

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.

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.

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.).

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

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.

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.

After the degradation of biological samples (e.g. milk, wool, etc.), it is often important to know the cystine/cysteine ratio. This Application Bulletin describes the simultaneous, polarographic determination of the two amino acids. The determination is performed in perchloric acid solution at the DME. Samples with a high protein content require that the determination is performed in an alkaline solution.

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.

This Bulletin describes a simple method for the determination of the calcium content in dairy products. The use of CuEGTA and the ion-selective copper electrode (Cu ISE) as indicator electrode allows the determination to be performed without time-consuming sample preparation. If the complexing agent EDTA is used as titrant instead of EGTA, the sum of calcium and magnesium is obtained. The magnesium content can then be calculated from the difference between the results of the two titrations.

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 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.

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

Determination of sodium, potassium, calcium, and magnesium in instant baby milk powder using cation chromatography with direct conductivity detection and dialysis for sample preparation.

Whey is the remaining liquid after cheese production. It is mainly used as feed. It is also used as dietary supplement as a beverage or in powder form. This application determines lactic acid as well as cations in one determination. The Metrosep C 6 - 250/4.0 column separates sodium, potassium, magnesium, and calcium by ion exchange. It also acts as an ion-exclusion column, which separates lactic acid. Both lactic acid and the cations can be determined in the same run applying direct conductivity detection. While cations typically elute as negative peaks, lactic acid elutes as an early positive peak. MagIC Net shows both in the usual positive direction.

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.

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

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

In the food industry, it is essential to determine and monitor certain quality parameters to guarantee consistency. This is especially important for liquid dairy products, which are subject to a strict cold chain. Both the dissolved oxygen (DO) and the pH value have proven to be reliable quality criteria. Oxygen shortens the shelf life and influences the product quality (e.g., nutritional value, color, and flavor). The DO content depends on the salinity in the sample, which is automatically calculated and corrected by the 914 pH/DO/Conductometer during the parallel conductivity measurement. Acidity is another important characteristic to measure that can be checked easily using the pH value. With the 914 pH/DO/Conductometer, all important quality criteria can be monitored with one device.

The water content of yoghurt powder is determined according to Karl Fischer. Because of the relatively high water and fat content, the sample is prediluted with a 1:1 mixture of chloroform and methanol.

This Application Note shows how easy it is to determine water content in the pharmaceutical excipient lactose with reagent-free near-infrared spectroscopy.

Lactose intolerance means that lactose cannot be digested. Lactose is contained in milk and milk products. "Lactose-free milk" is analyzed following Inline Dialysis. No lactose was detected in the milk sample investigated. The chromatogram of the spiked sample corresponds to the limit value of 100 mg/L that applies for lactose-free milk. The separation is performed on the Metrosep Carb 2 - 150/4.0 column.

EU Regulation 1169/2011 defines rules for nutrition declaration on foodstuffs. The objective is to provide food information to the general public and to label food ingredients that are hazardous to health when consumed in larger quantities. This Application Note describes the determination of fruit yogurt with the aid of the Metrosep Carb 2 - 150/2.0 column.

Iodine is an essential mineral for human health, where it is necessary for e.g., the production of thyroid hormones. The presented method describes the determination of free iodide in milk samples using Metrohm Low Volume Inline Dialysis for automated sample preparation prior to injection into an ion chromatograph (IC) and subsequent amperometric detection in direct current (DC) mode.

This Application Note presents ion chromatography with pulsed amperometric detection as fast and reliable method to determine low level lactose in complex matrices such as infant formula.

Worldwide, milk and dairy products are vital sources for human nutrition. A major component and energy source in dairy products is lactose. To efficiently metabolize lactose, the enzyme lactase is indispensable. However, globally nearly 70% of the population is lactose intolerant and they have difficulties to digest lactose. Lactose malabsorption leads to numerous gastrointestinal and extra-intestinal symptoms and other complaints with varying extents. Therefore, consumers rely on accurate food labels and for manufacturers appropriate sensitive analytical techniques are a must to comply with these demands. Ion chromatography with pulsed amperometric detection (IC-PAD) enables the determination of very low lactose contents. Validation according to AOAC requirements shows the high sensitivity and reliability of this method as a routine analysis.

Oxidation stability is an important quality criterion of chocolate as it provides information about the long-term stability of the product. Cocoa contains various flavonoids that act as antioxidants. The most important and common flavonoids are catechin, epicatechin, and procyanidin. Although the flavonoid content may vary amongst chocolate type, it can be said, the greater the cocoa content in the chocolate, the greater the antioxidant effect.Chocolate cannot be measured directly with the classical Rancimat method, as no evaluable induction time is obtained. There are many reasons for this, for example a too low fat content or various matrix effects. Traditionally, extraction of the fat from the chocolate using e.g., petroleum ether is therefore necessary.In this Application Note, the oxidation stability of white, milk and dark chocolate with varying cacao content is determined in without extraction. Instead, polyethylene glycol is used as conducting medium. More information on the Rancimat method can be found on the Metrohm website.

In 2008, a scandal was discovered in China that melamine was being deliberately added to raw milk. Thousands of young children and infants that consumed formula produced from melamine-tainted milk experienced kidney damage and death. As a result, both daily intake limits and increased monitoring of melamine in dairy products were established globally.Misa (Metrohm Instant SERS Analyzer) provides quick, easy, and robust detection of melamine in a complex food matrix. As a direct test with no additional reagents, Misa’s assay format requires minimal user training, in contrast to standard analytical tests for detecting melamine, including capillary electrophoresis, GC-MS, LC-MS, and immune-based assays.

Determination of iodide in milk powder using anion chromatography with conductivity detection after chemical suppression and inline sample preparation by dialysis.

Anion analysis in milk requires a sophisticated sample preparation to avoid column fouling by fats or proteins. Here Metrohm Inline Dialysis is the perfect automated technique. In dairy products iodide, thiocyanate, and perchlorate need to be determined regularly for health and hygiene reasons. This application allows for the first time to analyze these three components in this matrix within one run.

Determination of calcium in cheese by potentiometric titration with EGTA using the Cu-ISE.

In this Application Note, the determination of calcium in milk is shown with the copper ion-selective electrode which is less sensitive to contamination from proteins.

The titratable acidity gives an indication of the freshness of milk and yogurt as well as other fermented milk products. The determined titratable acidity in milk is mainly given through the absorption of hydroxyl ions by milk proteins and milk salts. The acidity increases with bacterial acidification and with enzymatic lipolysis. The titratable acidity corresponds to the amount of sodium hydroxide required to titrate 100 g sample to a pH value of 8.30.In this Application Note, an easy and accurate method to determine the titratable acidity in milk according to DIN 10316 and in yogurt according to ISO/TS 11869 and IDF/RM 150 is demonstrated.

In order to maintain product quality, the sodium chloride content in dairy products must be monitored and not exceed the limits defined by the respective public health authorities. The chloride content in food correlates with the salt content, its determination is therefore described in various norms and standards. However, preparation of such samples is time consuming, as it includes a chloride extraction with warm water. Whole milk powders in particular are difficult to handle as an inhomogeneous dispersion of fat in the titration suspension occurs.In order to reduce the workload, increase sample throughput, and eliminate the matrix challenges posed by high fat products, this Application Note presents a fully automatic potentiometric titration of chloride with silver nitrate in milk and milk powder based on ISO 21422, IDF 242, AOAC 2015.07, AOAC 2015.08 and AOAC 2016.03

The salt content in food is a critical parameter, given that the WHO recommends a maximum daily intake of 5 g for an adult. In butter with a salt content exceeding 0.1%, it can be determined by a precipitation titration of chloride with silver nitrate. However, during manual titration the operator cannot leave the system unattended because he has to exchange the sample beakers manually which is time consuming and prone to errors.This Application Note describes the automated determination of chloride in salted butter in accordance with ISO 15648, ISO 21422, IDF 179 and IDF 242. If automated according to the norms and standards, salt determination can be performed completely unattended with superior reproducibility of results increasing efficiency in the laboratory.

The WHO recommends a maximum daily intake of 5 g salt for an adult. The chloride content in food correlates with the salt content, its determination is therefore described by various standards. In cheese and cheese products with a chloride content higher than 0.2%, chloride is usually determined by a precipitation titration with silver nitrate. However, time-consuming sample preparation is required, as the cheese has to be homogenized and the chloride extracted with hot water.This Application Note describes the fully automatic determination of chloride in cheese according to EN ISO 5943, ISO 21422, IDF 242 and IDF 88 including sample preparation with a Polytron homogenizer. This increases productivity due to a higher sample throughput and lower work load for the operator.

Vitamin C is an important antioxidant included in milk powder. The double Auring electrode provides an excellent titration curve when using 2,6-dichlorophenolindophenol (DPIP) as titrant and is easy to clean.With the OMNIS system, a fast and accurate determination of vitamin C in milk powder by a bi-voltametric titration is realized.

Determination of melamine in milk, diary products, eggs, and egg-based foodstuffs using cation chromatography.

Determination of cysteine and cystine in caseinate after sample preparation with NaOH.

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

This article describes the fully automated ion chromatography determination of chloride, phosphate and sulfate in an ultraheat-treated (UHT) milk sample and baby milk powder dissolved in water by means of the 881 Compact IC pro ion chromatograph and the upstream Metrohm dialysis cell.

Table salt (sodium chloride) is added to many foods as a preservative and flavor enhancer. Precise and accurate analyses are required for quality monitoring. Determination with thermometric titration is simpler and less expensive than with spectroscopy, and the entire process can be automated.This article uses various foods as examples for showing how simple, rapid and precise sodium determination with thermometric titration is.