Filtro de Aplicações

Quantitation of the functionalization of a water-soluble polymer was achieved using a portable Raman spectrometer. The Raman spectrum provides strong, unique bands for both the initial and fully reacted polymer. This enables development of a simple, robust quantitative analysis of the percent polymer functionalization. This method is now routinely used in a manufacturing plant's quality control laboratory.

Metal precipitation and cyanide recovery in the SART process (sulfidization, acidification, recycling, thickening) depend to a great extent on the sulfide concentration. Among the flow injection analysis methods coupled to wet-chemical analyzers, the combination of a gas diffusion cell with an ion chromatograph (IC) plus subsequent direct spectrophotometric detection has proven to be one of the most convenient methods of sulfide analysis.This paper deals with the determination of sulfide anions via the coupling of a gas diffusion cell to an IC with subsequent spectrophotometric detection.

This poster describes a simple and sensitive method for the determination of perfluorooctanoate (PFOA) and perfluorooctane sulfonate (PFOS) in water samples by suppressed conductivity detection. Separation was achieved by isocratic elution on a reversed-phase column thermostated at 35 °C using an aqueous mobile phase containing boric acid and acetonitrile. The PFOA and PFOS content in the water matrix was quantified by direct injection applying a 1000 μL loop. For the concentration range of 2 to 50 μg/mL and 10 to 250 μg/mL, the linear calibration curve for PFOA and PFOS yielded correlation coefficients (R) of 0.99990 and 0.9991, respectively. The relative standard deviations were smaller than 5.8%.The presence of high concentrations of mono and divalent anions such as chloride and sulfate has no significant influence on the determination of the perfluorinated alkyl substances (PFAS). In contrast, the presence of divalent cations, such as calcium and magnesium, which are normally present in water matrices, impairs PFOS recovery. This drawback was overcome by applying Metrohm`s Inline Cation Removal. While the interfering divalent cations are exchanged for non-interfering sodium cations, PFOA and PFOS are directly transferred to the sample loop. After inline cation removal, PFAS recovery in water samples containing 350 mg/mL of Ca2+ and Mg2+ improved from 90…115% to 93…107%.While PFAS determination of low salt-containing water samples is best performed by straightforward direct-injection IC, water rich in alkaline-earth metals are best analyzed using Metrohm`s Inline Cation Removal.

UV/VIS detection is one of the most sensitive detection techniques in trace-level chromatography. Sometimes, however, spectrophotometric detection lacks sensitivity, selectivity or reproducibility and chemical derivatizations are required. By using Metrohm`s rugged and versatile flow-through reactor, single- or multi-step derivatizations can be done fully automatically, in either pre- or post-column mode at any temperature between 25…120 °C. The variable reactor geometry allows to adjust the reactor residence time of the reactants according to derivatization kinetics. The flexibility of the reactor is demonstrated by optimizing four widespread post-column techniques: the relatively slow ninhydrin reaction with amino acids and the fast derivatizations of silicate, bromate and chromate(VI).

This poster discusses results showing the influence of pH, temperature of the post-column reactor, eluent composition, and iodide concentration on the sensitivity of the triiodide method.

The determination of cyanide is very important not only in electroplating baths and when decontaminating wastewater but, due to its high toxicity, also in water samples in general. Concentrations of 0.05 mg/L CN- can already be lethal for fish. This Bulletin describes the determination of cyanide in samples of different concentrations by potentiometric titration. Chemical reactions: 2 CN- + Ag+ → [Ag(CN)2]- [Ag(CN)2]- + Ag+ → 2 AgCN

The photometric determination of nitrate is limited by the fact that the respective methods (salicylic acid, brucine, 2,6-dimethyl phenol, Nesslers reagent after reduction of nitrate to ammonium) are subject to interferences. The direct potentiometric determination using an ion-selective nitrate electrode causes problems in the presence of fairly large amounts of chloride or organic compounds with carboxyl groups. The polarographic method, on the other hand, is not only more rapid, but also practically insensitive to chemical interference, thus ensuring more accurate results. The limit of quantification depends on the matrix of the sample and is approximately 1 mg/L.

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 document explains how to measure Na ion concentration in diverse matrices with a sodium ion-selective electrode (Na-ISE) using direct measurement and standard addition.

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).

This Bulletin describes the complexometric potentiometric titration of metal ions. An ion-selective copper electrode is used to indicate the endpoint of the titration. Since this electrode does not respond directly to complexing agents, the corresponding Cu complex is added to the solution. With the described electrode, it is possible to determine water hardness and to analyze metal concentrations in electroplating baths, metal salts, minerals, and ores. The following metal ions have been determined: Al3+, Ba2+, Bi3+, Ca2+, Co2+, Fe3+, Mg2+, Ni2+, Pb2+, Sr2+, and Zn2+.

This Application Bulletin describes a polarographic method for the determination of cyanide that allows to determine free cyanide fast and accurately. The determination also succeeds in solutions containing sulfides, where other methods fail. Cyanide concentrations in the range b(CN–) = 0.01...10 mg/L cause no problems. Interference caused by anions and complexed cyanides has been investigated.

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.

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.).

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.

"A sensitive methods to determine manganese is described. It is primarily suitable for the investigation of ground, drinking and surface waters, in which the concentration of manganese is important. The method can naturally also be used for trace analysis in other matrices. Manganese is determined in an alkaline borate buffer by the anodic stripping voltammetry (ASV). Interference by intermetallic compounds is prevented by the addition of zinc ions in the sample. The limit of determination lies at b(Mn) = 2 µg/L."

This bulletin describes the determination of calcium, magnesium, and alkalinity in water by complexometric titration with EDTA as titrant. It is grouped into two parts, the potentiometric determination and the photometric determination. There are multiple definitions of the different types of water hardness. In this Application Bulletin, the following definitions are used: alkalinity, calcium hardness, magnesium hardness, total hardness, and permanent hardness. Explanations of these definitions and other expressions are provided in the Appendix. Determination of alkalinity during the photometric part is carried out in a separate acid-base titration before the complexometric titration of calcium and magnesium in water. Permanent hardness can be calculated from these values. The determination of calcium and magnesium in beverages (fruit and vegetable juices, wine) is also described. The photometric part includes the determinations of total and calcium hardness and thereby indirectly magnesium hardness using Eriochrome Black T and calconcarboxylic acid as indicators (in accordance with DIN 38406-3).

Nitrite can be determined polarographically after its conversion to diphenylnitrosamine (C6H5)2NNO. Potassium thiocyanate is used as a catalyst in order for the conversion to proceed rapidly and quantitatively. The reaction takes place in acid solution at a pH value of approx. 1.5. The limit of quantification is 5 μg/L NO2-.

After acid digestion, the sample solution is neutralized with sodium hydroxide to form sodium dihydrogen phosphate. An excess of lanthanum nitrate is added and the released nitric acid is then titrated with sodium hydroxide solution. NaH2PO4 + La(NO3)3 → LaPO4 + 2 HNO3 + NaNO3 This determination method is suitable for higher phosphate concentrations.

Besides acid-base titrations, the titrimetric determination of chloride is one of the most frequently used titrimetric methods of analysis. It is employed more or less frequently in practically every laboratory. This Bulletin shows you how to determine chloride in a wide range of concentrations using automatic titrators. Silver nitrate is normally used as titrant (for environmental reasons one should refrain from using mercury nitrate). The titrant concentration depends on the chloride content of the sample to be analyzed. It is crucial to choose the correct electrode for samples with low chloride contents.

This Application Bulletin describes a voltammetric method for the determination of aluminum in water samples, dialysis solutions, sodium chloride solutions and digestion solutions (e.g. of lyophilisates). The method utilizes the complexation of the Al3+ ion by Calcon (Eriochrome blue black R). The formed complex can easily be reduced electrochemically at 60 °C. The limit of quantitation depends on the purity of the reagents used and is approx. 5 µg/L.

"Molybdenum is an essential trace element for plant growth. Since it occurs in natural waters only in trace amount, a very sensitive method of determination is needed. Using the following polarographic method, it is possible to determine 5·10-10 mol/L resp. 50 ng/L. The principle of the method is based on the reaction between the molybdate ion MoO42- and the complexing agent 8-hydroxy-7-iodo-quinoline-5-sulfonic acid (H2L) to form a MoO2L22- complex, which is adsorbed on the mercury electrode. The adsorbed Mo(VI) is reduced electrochemically to the Mo(V) complex. The hydrogen ions present in the solution oxidize Mo(V) again spontaneously to form the Mo(VI) complex, which is thus newly available for electrochemical reduction. This catalytic reaction is the reason for the high sensitivity of the method. Tungsten W(VI) exhibits practically the same electrochemical behavior as molybdenum, but is not described in detail in this Application Bulletin."

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 200:1 According 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 determination of the physical and chemical parameters as electrical conductivity, pH value, p and m value (alkalinity), chloride content, the calcium and magnesium hardness, the total hardness, as well as fluoride content are necessary for evaluating the water quality. This bulletin describes how to determine the above mentioned parameters in a single analytical run. Further important parameters in water analysis are the permanganate index (PMI) and the chemical oxygen deman (COD). Therefore, this Bulletin additionally describes the fully automated determination of the PMI according to EN ISO 8467 as well as the determination of the COD according to DIN 38409-44.

This Bulletin describes the voltammetric determination of aluminum in water samples down to a concentration of 1 μg/L. An aluminum complex is formed with alizarin red S (DASA) and enriched at the HMDE. The following determination employs differential pulse adsorptive stripping voltammetry (DP-AdSV). Disturbing Zn ions are eliminated by addition of CaEDTA.

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.

Sulfide and sulfite can be determined polarographically without any problems. For sulfide, polarography is performed in an alkaline solution, for sulfite in a slightly acidic primary solution. The method is suitable for the analysis of pharmaceuticals (infusion solutions), wastewater/flue gas water, photographic solutions, etc.

This Application Bulletin describes the stripping analysis of Ag at the rotating disk electrode (RDE) with glassy carbon tip (GC) or Ultra Trace graphite tip. In routine operation, the determination limit lies at approx. 10 μg/L Ag, with careful work 5 μg/L Ag can be obtained. After appropriate digestion, silver determination is also possible with samples containing a relatively high proportion of organic substances (e.g. wine, foodstuffs etc.). The method has been developed primarily for water samples (well, ground and wastewater, desilvering solutions of the photographic industry).

This Application Bulletin describes …

This Bulletin describes the determination of arsenic by anodic stripping voltammetry (ASV) at the rotating gold electrode. A determination limit of 0.5 μg/L can be achieved with 10 mL sample solution. A differentiation between the As(III) concentration and the total arsenic concentration can be made by appropriate selection of the deposition potential. The analyses are performed with a special gold electrode whose active surface is located laterally; c(HCl) = 5 mol/L is used as supporting electrolyte. For the determination of the total arsenic content, As(III) and As(V) are reduced at -1200 mV by nascent hydrogen to As0, which is preconcentrated on the electrode surface. If the deposition is carried out at -200 mV then only As(III) is reduced; this allows the differentiation between total arsenic and As(III). During the subsequent voltammetric determination the preconcentrated As0 is again oxidized to As(III).

The titrimetric determination of nonionic surfactants on the basis of polyoxyethylene adducts (POE adducts) is described in the Bulletin. The basis for the determination is the transfer of the nonionic surfactant into a pseudo-cation compound and its precipitation titration with sodium tetraphenylborate (Na-TPB). The NIO electrode is used for the indication of the potentiometric titration. This Bulletin describes determinations in raw products, formulations and wastewater and draws attention to special features, possibilities, limits and disruptions.

This Application Bulletin describes the determination of cadmium and lead at a mercury film electrode (MFE) by anodic stripping voltammetry (ASV). The mercury film is plated ex situ on a glassy carbon electrode and can be used for up to one day. With a deposition time of 30 s, the limit of detection is ß(Cd2+) = 0.02 µg/L and ß(Pb2+) = 0.05 µg/L. The linear working range for both elements goes up to approx. 50 μg/L using the same deposition time.

The method described allows the determination of W(VI) traces in the range 0.2 to 50 µg/L (ppb). Traces of organic compounds present in the samples (e.g. natural waters) interfere. They have to be removed by UV digestion (e.g. 705 UV Digester). Interference by Fe(III) up to a concentration of 100 mg/L is eliminated by reduction to Fe(lI) with ascorbic acid. If the amount of Cu(II) in the sample exceeds the amount of W(VI) by a factor of 200 or more, the Cu ions have to be bound with thiourea. Moreover, the concentration of Cu(II) should not exceed 5 mg/L. The determination is made by adsorptive stripping analysis in the DP mode.

The method describes the determination of Cr traces in a range between 1 ... 250 μg/L. The method is based on the adsorption of a Cr(lll)-diphenylcarbazonate complex on the Ultra Trace graphite rotating disk electrode (RDE). Organic compounds present in samples (e.g. natural waters) have a strong interfering effect. So they have to be removed by e.g. UV digestion. The determination is made by adsorptive stripping voltammetry in the DC (direct current) measuring mode. Purging with nitrogen is not necessary. The determinations work well also in high salt concentration solutions.

This Application Bulletin describes the determination of zinc at a mercury film electrode (MFE). Zinc can also be determined simultaneously with cadmium and lead. The determination of copper at the MFE is not possible. The mercury film is plated ex-situ on a glassy carbon electrode and can be used for half a day up to one day. Zinc can be determined at the mercury film electrode by anodic stripping voltammetry (ASV). The presence of copper, which is naturally present in many samples, affects the determination of zinc due to the formation of an intermetallic compound. As a result the determined concentrations of zinc are too low. The addition of gallium can eliminate the interference to a certain extent since the intermetallic complex of gallium and copper is more stable than the complex of zinc and copper. With a deposition time of 10 s, the limit of detection is β(Zn2+) = 0.15 μg/L. The linear working range goes up to approx. 300 μg/L.With the deposition time of 10 s the method is suitable for samples between 10 μg/L and 150 μg/L Zn content. For samples with lower concentrations the results are more reliable if the deposition time is increased to e.g. 30 s. Samples with higher concentrations have to be diluted.

This Application Bulletin describes the determination of titanium by adsorptive stripping voltammetry (AdSV) using mandelic acid as complexing agent. The method is suitable for the analysis of ground, drinking, sea, surface and cooling waters, in which the concentration of titanium is of importance. The methods can, of course, also be used for the trace analysis in other matrices. The limit of detection is approx. 0.5 µg/L.

This Application Bulletin describes two methods for the determination of iron at the Multi Mode Electrode. Method 1, the polarographic determination at the DME, is recommended for concentrations of β(Fe) > 200 μg/L. For this method the linear range is up to β(Fe) = 800 μg/L. For concentrations < 200 μg/L Method 2, the voltammetric determination at the HMDE, is to be preferred. The detection limit for this method is β(Fe) = 2 μg/L, the limit of quantification is β(Fe) = 6 μg/L. The sensitivity of the method cannot be increased by deposition. Iron(II) and iron(III) have the same sensitivity for both methods. These methods have been elaborated for the determination of iron in water samples. For water samples with high calcium and magnesium concentrations such as, for example, seawater, a slightly modified electrolyte is used in order to prevent precipitation of the corresponding metal hydroxides. The methods can also be used for samples with organic loading (wastewater, beverages, biological fluids, pharmaceutical or crude oil products) after appropriate digestion.

This Application Bulletin describes the determination of arsenic in water samples by anodic stripping voltammetry using the scTRACE Gold sensor. This method makes it possible to distinguish between As(total) and As(III). With a deposition time of 60 s, the limit of detection for As(total) is 0.9 µg/L, for As(III) it is 0.3 µg/L.

This Application Bulletin describes the determination of inorganic mercury in water samples by anodic stripping voltammetry using the scTRACE Gold sensor. With a deposition time of 90 s, calibration is linear up to a concentration of 30 µg/L; the limit of detection lies at 0.5 µg/L.

This Application Bulletin describes the methods for the determination of uranium by adsorptive stripping voltammetry (AdSV) according to DIN 38406 part 17. The method is suitable for the analysis of ground, drinking, sea, surface and cooling waters, in which the concentration of uranium is of importance. The methods can, of course, also be used for the trace analysis in other matrices. Uranium is determined as chloranilic acid complex. The limit of detection in samples with low chloride concentration is about 50 ng/L and in seawater about 1 µg/L. Matrices with high chloride content can only be analyzed after reduction of the chloride concentration by means of a sulfate-loaded ion exchanger.

This Application Bulletin describes the voltammetric determination of the elements iron, copper and vanadium. Fe as well as Cu and V can be determined as catechol complex at the HMDE by adsorptive stripping voltammetry (AdSV). Fe(II) and Fe(III) are determined as Fe(total) with the same sensitivity for both species in either phosphate buffer or PIPES electrolyte. Cu and V can be determined in PIPES buffer. The methods are primarily suitable for the investigation of ground, drinking and surface waters, in which the concentration of these metals is important. But the methods can naturally also be used for trace analysis in other matrices. The limit of detection for all three elements in PIPES buffer is 0.5 ... 1 µg/L, for iron in phosphate buffer it is approx. 5 µg/L.

Lead is known to be highly toxic and lead salts are easily absorbed by creatures. By interfering with enzyme reactions, lead can affect all parts of the human body. It can cause severe damage to brain and kidneys and can cross the bloodbrain barrier. Cases of chronic lead poisoning caused by lead metal used in the water piping system are well known. Therefore, the control of drinking water for lead content is of utmost importance. In many countries (e.g., EU, USA), the limit for lead in drinking water is between 10 and 15 μg/L. These concentrations can reliably be determined with the method described in this Application Bulletin. The determination is carried out by anodic stripping voltammetry at a silver film applied to the scTRACE Gold electrode.

EC-SERS enhances Raman sensitivity using electrochemically activated gold SPEs, enabling rapid, simplified pesticide detection without complex prep or instrumentation.

Determination of lithium, sodium, potassium, magnesium, and calcium in lake water using cation chromatography with direct conductivity detection.

Cation content in snow is greatly dependent on sampling site. Samples from remote areas are expected to exhibit lower cation concentrations. This application shows the analysis of a snow sample from an open field in an agricultural zone. Separation is performed on a microbore Metrosep C 6 - 100/2.0 column with direct conductivity detection. The relatively high ammonia content can be explained by animal husbandry in the vicinity of the sampling site.

Cation content in snow is greatly dependent on sampling site. Roadside samples are likely to exhibit a high sodium content caused by the use of road salt. This application shows the analysis of a snow sample from a roadside. Separation is performed on a microbore Metrosep C 6 - 250/2.0 column with direct conductivity detection. The 250 mm column was selected due to the large difference in concentrations between sodium and ammonia. This condition enables a baseline separation of the two cations.

Combustion ion chromatography (CIC) measures AOX (adsorbable organically bound halogens, i.e., AOCl, AOBr, AOI) and AOF as well as CIC AOX(Cl) according to DIN 38409-59 and ISO 18127.

Tafel analysis is an important electrochemical technique used to understand reaction kinetics. By studying the Tafel slope, it reveals the rate-determining steps in electrode reactions, aiding fields like corrosion and fuel cell research. This method helps industries optimize processes and improve device performance by tailoring materials and conditions for greater efficiency.

With the advent of electric automobiles, the demand for lithium batteries and with it the demand for lithium material will increase sharply. Brine lakes and hard silicate minerals are numbered among the most important sources of lithium. This Application Note addresses cation determination in seepage water from lithium minerals. Alkali and earth alkali metals are separated in the lithium digestions on the Metrosep C Supp 1 - 250/4.0 column, with subsequent conductivity detection after sequential suppression.

Sequential suppression in cation chromatography significantly improves detection limits. The determination of the blank value of the sample vial being used is thus essential for being able to achieve such low detection limits. The leaching tests of various sample vials proceed with the intelligent Preconcentration Technique with Matrix Elimination on the Metrosep C Supp 1 - 250/4.0 column with conductivity detection following sequential suppression. The 50 mL Corning® Cell Culture Flasks from Sigma-Aldrich (CLS430168) exhibit the lowest blank values.

The determination of heavy metal ions in a solution is one of the most successful application of electrochemistry. In this application note, anodic stripping voltammetry is used to measure the presence of two analytes, in a sample of tap water.

This Application Note presents a walkthrough of an experiment on 4-nitrothiophenol using hyphenated EC-Raman, a combination of Raman spectroscopy and electrochemistry.

Advances in polymeric membranes and screen-printed technologies have enabled miniaturized, portable potentiometric sensors ideal for point-of-care analysis.

Spectro electrochemiluminescence experiments comparing photodiode and microspectrometer detectors, showing how each sensor captures ECL signals for the analysis of single and dual luminophore systems.

Alamar Blue is monitored with fluorescence spectroelectrochemistry during its irreversible reduction to resorufin and further reversible reduction to dihydroresorufin.

Even in low concentration, sulfide ions cause odor and corrosion problems in ground water and waste water. They can release hydrogen sulfide in acidified water, which is toxic in even minuscule amounts. This Application Note describes the determination of sulfide concentration in water via direct measurement with the Ag/S-ISE in accordance with ASTM D4658.

Bromide is ubiquitous in sea water, where it is present in concentrations of around 65 mg/L. By contrast, the maximum bromide concentration in drinking and ground water is usually less than 0.5 mg/L. A higher bromide content may indicate a contamination of the water caused by fertilizer, road salt or industrial waste water. This Application Note describes the determination of the bromide content in water via direct measurement with a Br ion-selective electrode in accordance with ASTM D1246.

Oxygen diffuses into water sources from the air via aeration, however several factors can reduce the dissolved oxygen (DO) content in water. First, as water warms up, oxygen is released into the atmosphere. Secondly, oxygen is consumed by bacteria and other microorganisms which feed on organic material. Finally, plants can also consume oxygen in certain situations. Human-induced alterations can have a negative influence on surface water when DO values fall below crucial limits for maintaining the life supporting capacity of freshwater ecosystems. Therefore, monitoring the DO content in surface water by an optical sensor to assess its quality is important.

In municipal water supplies, higher dissolved oxygen (DO) content is desirable because it improves the taste of drinking water. However, high DO levels also speed up corrosion in water pipes. For this reason, industries utilize water with as little DO as possible, and add scavengers such as sodium sulfite to remove any oxygen from a water supply. Municipal water supply pipes are normally coated inside with polyphosphates to protect the metal from contact with oxygen, thus allowing higher DO contents. Therefore, monitoring the DO content online in a water supply is important to assess its DO content to either improve taste or minimize pipe corrosion. Using an optical sensor, such as the O2-Lumitrode, allows a fast and reliable determination according to ISO 17289.

This Application Note covers the formation of calcium carbonate from solution.

Perchlorate contamination in drinking water may have different sources. Besides natural deposits, anthropogenic sources like fertilizers and rocket fuel residue add to hazardous water contamination. Perchlorate interferes with iodine uptake into the thyroid gland. Newborns and children are particularly vulnerable, affected as thyroid hormones are essential for growth. Besides ion chromatography (IC) followed conductivity detection, IC hyphenated with an MS detector can be used to measure perchlorate down to sub-µg/L levels. In this application IC is hyphenated with a triple-quadrupole MS (IC-MS/MS) for perchlorate determination in order to meet the requirements of EPA 332.0. This IC-MS/MS setup avoids the possible interference of sulfate.

The new DIN draft standard 38407-53 outlines TFA analysis in water using direct injection LC-MS/MS, enabling quantification from 0.1–3.0 μg/L as shown in this Application Note.

Determination of traces of bromide and iodide using anion chromatography with amperometric detection at the silver electrode.

Determination of chromate using anion chromatography with post-column reaction and UV/VIS detection.

Determination of silicate and borate and their limits of determination (LOD) and quantification (LOQ) according to the EPA procedure for method detection limit (MDL) using anion chromatography with direct conductivity detection and Metrohm Inline Calibration.

Determination of sodium dodecylsulfate (SDS, sodium laurylsulfate) using anion chromatography with direct conductivity detection.

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.

The combination of 940 Professional IC Vario, 942 Extension Module Vario LQH and 941 Eluent Preparation Module enables process monitoring with the aid of ion chromatography. Assigned the designation ProfIC Vario 12 Anion, this combination is the anion variant of Metrohm Process IC. Intelligent preconcentration technology with matrix elimination is used for sample preparation. The use of an ELGA PURELAB® Flex 6 guarantees the supply of ultrapure water of the highest quality, particularly in cases of high numbers of samples.

Low sensitivity has limited the use of Raman spectroscopy as a detection method. However, the surface-enhanced Raman scattering (SERS) effect has improved its effectivity for analytical use. Aldehyde dehydrogenase (ALDH) and cytochrome c are analyzed by Raman spectroelectrochemistry as a proof of concept in this Application Note.

Malachite green (MG) is a textile dye with effective fungicidal properties, however it is acutely toxic and its metabolites persist in the flesh of fish and mammals, making it a threat to the human food chain. The EU has concluded that contaminated foods containing levels higher than 2 μg/g MG constitute a credible health risk, and several countries have banned malachite green as an aquaculture additive. Despite tight regulation, seafood products contaminated with MG continue to find their way to consumers. Using Misa (Metrohm Instant SERS Analyzer) to ensure food safety, the rapid and highly sensitive detection of malachite green is achieved in a facile assay format.

Determination of fluoride, chloride, nitrite, bromide, nitrate, and sulfate in surface water using anion chromatography with conductivity detection after chemical suppression.

Determination of fluoride, chloride, nitrate, phosphate, and sulfate in surface water using anion chromatography with conductivity detection after chemical suppression; nitrite with electrochemical detection (conductivity and ELCD detectors in series).

Determination of NTA, EDTA, and DTPA in surface water and wastewater using ion pair chromatography with UV-detection after post-column reaction with the MSM.

Determination of fluoride, chloride, nitrite, nitrate, and sulfate in rainwater using anion chromatography with conductivity detection after chemical suppression.

Determination of chlorite and nitrite using anion chromatography with amperometric detection at the carbon paste electrode after chemical suppression.

Determination of acetate, propionate, formate, and chloride in water using anion chromatography with conductivity detection after chemical suppression.

Determination of NTA, HEDP, and ATMP using anion chromatography with conductivity detection after chemical suppression.

Determination of fluoride, chloride, nitrite, bromide, nitrate, phosphate, sulfite, and sulfate in river water using anion chromatography with conductivity detection after chemical suppression.

Determination of 2-fluorobenzoate in a water deposit from the oil production industry using anion chromatography with conductivity detection and chemical suppression.

Determination of fluoride, chloride, nitrite, bromide, nitrate, phosphate, and sulfate in water from an agricultural irrigation system using anion chromatography with conductivity detection after chemical suppression.

Determination of perchlorate in water containing 3 g/L of total dissolved solids (TDS) using anion chromatography with conductivity detection after chemical suppression.

Fast and reliable analysis of drinking water by combining EPA method 300.1 Parts A and B in a single IC run.

Determination of fluoride, chloride, nitrate, phosphate, and sulfate on a short column or the ions mentioned plus bromate and nitrite on a long column in water samples applying intelligent column-switching using anion chromatography with conductivity detection after sequential suppression.

Swimming pool water needs to be thoroughly disinfected and this is often accomplished with ozonization. This process can generate harmful oxyhalides, the concentration of which must be monitored. Here the separation and determination of oxyhalides as well as standard anions are carried out using a column of the Metrosep A Supp 5 - 250/4.0 type. Quantification takes place using conductivity detection in accordance with sequential suppression.

EN ISO 10304-1 is one of the most important standards for the determination of the seven standard anions in water samples. Many other standards refer to EN ISO 10304-01 if anion determination by IC is required. This standard asks for a membrane filtration for samples to avoid bacteria and solids, if required. This application shows the determination of anions according EN ISO 10304-1 applying Inline Ultrafiltration. This setup avoids tedious manual sample filtration and handles any samples fully automatically.

The Metrosep A Supp 21 column and 948 Continuous IC Module, CEP enable efficient, automated single-run analysis of major anions and disinfection byproducts in water.

Spectroelectrochemical experiments not only provide outstanding qualitative information about samples, but also offer other quantitative data that can be considered when performing analyses. A single set of experiments allows analysts to obtain two calibration curves: one with the electrochemical data and another with the spectroscopic information. The concentration of tested samples is calculated by using both curves, confirming the obtained results by two different routes. In this Application Note, comparison between electrochemical and spectroscopic determinations demonstrates that the two methods measure uric acid (UA) indistinctively, with close agreement of the calculated values with empirical data.

The development of a novel reflection cell for conventional electrodes facilitates the performance of spectroelectrochemical measurements. This device allows researchers to work in aqueous solutions as well as in organic media due to its chemical resistance.

Poly(3,4-ethylenedioxythiophene) (PEDOT) is one of the most promising ICPs due to its high conductivity, electrochemical stability, catalytic properties, high insolubility in almost all common solvents and interesting electrochromic properties (transparent in the doped state and colored in the neutral state). In this Application Note, PEDOT film is evaluated by spectroelectrochemical techniques.

This Application Note presents a potentiometric titration method for trace H2S analysis in water on an OMNIS system using silver nitrate and an Ag Titrode.

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.

Alkalinity is well-suited as a means of describing the capacity of a body of water to neutralize acid contaminations. It is therefore an important indicator for estimating the influence of contaminations on the ecological system.

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.

Water treatment with ozone (O3) is a common procedure for the disinfection of swimming pools. It is important that a sufficient but not excessive amount of O3 is produced to disinfect the water. Otherwise, the remaining ozone could enter the swimming water, which could irritate the respiratory system or the skin of bathers. Ozone is also used in drinking and waste water treatment because it is significantly more effective than chlorine at inactivating or killing viruses and bacteria. This application note describes a method to determine the ozone concentration in water by potentiometric titration according to DIN 38408-3.

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.

Chromate and dichromate are the two oxoanions of chromium. In both, chromium is present in its hexavalent form (Cr(VI)). In aqueous solutions, chromate exists under alkaline and dichromate under acidic conditions. Hexavalent chromium is highly toxic and carcinogenic. It is therefore restricted in manufactured goods as well as in the environment and requires thorough monitoring. DIN 38405-52 describes the determination of Cr(VI) in water, wastewater, and sludge by photometric methods. In Appendix C, chapter C.6 the use of ion chromatography is described. This AN shows the application of the method to drinking water samples.

The combination of ion chromatography and inductively coupled plasma mass spectrometry (IC-ICP/MS) is ideally suited for the detection of species of arsenic and mercury in their various oxidation levels and forms of chemical bonding. However, some species – as in the case of mercury – are reciprocally converted into one another during sample preparation, thus making a determination of the initial concentrations of the heavy metal species impossible. This article shows how these interconversions can be calculated with isotope dilution analysis and IC-ICP/MS in accordance with EPA method 6800.

The coupling of ion chromatography and inductively coupled plasma mass spectrometry (ICP/MS) leads to a high-performance measurement system that masters several particularly challenging analyses. It enables for example reliable determination of element compositions, oxidation states and chemical bonds. This information is used, for example, for assessing the toxicity of medications, environmental and water samples as well as foods and beverages.

Brad Meadows is Vice President and Lab Director at the US company BSK Labs, which runs a number of environmental laboratories and service centers. Brad is an analytical chemist and has been working in the management of analysis laboratories for 15 years. He shared his experiences with Metrohm ion chromatography with us in the form of some concrete facts and figures.

Heavy metals such as arsenic and mercury find their way into the ground water in many regions of the world, either through natural processes or as the result of human activities. Limit values are exceeded many times over, particularly for arsenic in drinking water, in many areas. This calls for a rigorous monitoring of water quality. The present whitepaper focuses on field determinations of arsenic, mercury, and copper – directly at the sampling site.

Electrochemical measurements utilizing a rotating cylinder electrode (RCE) are widely used in industrial corrosion applications when simulation of realistic pipe conditions are necessary in a lab environment. This white paper allows further insight into the particularities and parameters which govern the electrochemical measurements, in particular measurements performed in turbulent flow conditions, and shows a complete picture of the best practice use of this technique. The annexes provide an overview and short explanation of the parameters and laws specific to the fluid behavior in electrochemical cells with RCE.

«Dissolved oxygen» describes the amount of oxygen molecules (O2) which are dissolved in a liquid phase under certain conditions. In this white paper, two different methods for the analysis of dissolved oxygen, titration and direct measurement, are compared and contrasted to help analysts determine which method is more suitable for their specific applications. Here, we primarily focus on the determination of dissolved O2 in water. However, the same principle applies for other liquid phases such as non-alcoholic or alcoholic beverages.

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.

Ion chromatography mass spectrometry (IC-MS) is a powerful tool that can handle many challenging analytical tasks which cannot be performed adequately by IC alone. IC-MS is a robust, sensitive, and selective technique used for the determination of polar contaminants like inorganic anions, organic acids, haloacetic acids, oxyhalides, or alkali and alkaline earth metals. After separation of the sample components via IC, mass selective detection guarantees peak identity with low detection limits. The inclusion of automated Metrohm Inline Sample Preparation (MISP) allows not only water samples, but also chemicals, organic solvents, or post-explosion residues to be readily analyzed without need for extensive manual laboratory work. This White Paper explains the benefits of IC-MS over IC in certain cases, the hyphenation of IC and different MS systems, as well as related norms and standards.

Learn about PFAS, their impact on water quality, EU Directive 2020/2184, and the benefits of AOF measurement using combustion ion chromatography (CIC).

This White Paper presents four different «green» sensors: the scTRACE Gold, screen-printed electrodes, the glassy carbon electrode, and the Bi drop electrode from Metrohm that can be used to determine low concentrations of heavy metals in different sample matrices, such as boiler feed water, drinking water, and sea water.

The ASTM D8192 standard allows analysts to determine water hardness in different water matrices by complexometry with automated photometric endpoint recognition, increasing the reproducibility and the precision of the results.