Applications

Research laboratories must expand their capabilities to routinely analyze candidate microplastics from environmental samples to determine their origin and help predict biological impacts. Spectroscopic techniques are well suited to polymer identification. Laboratory Raman spectroscopy is an alternative to confocal Raman microscopes and Fourier transform infrared (FTIR) microscopes for quick identification of polymer materials. Raman microscopy was used to identify very small microplastic particles in this Application Note.

The coupling of highly efficient ion chromatography (IC) to multi-dimensional detectors such as a mass spectrometer (MS) or an inductively coupled plasma mass spectrometer (ICP/MS) significantly increases sensitivity while simultaneously reducing possible matrix interference to the absolute minimum. By means of IC/MS several oxyhalides such as bromate and perchlorate can be detected in the sub-ppb range. Additionally, organic acids can be precisely quantified through mass-based determination even in the presence of high salt matrices. By means of IC-ICP/MS different valence states of the potentially hazardous chromium, arsenic and selenium in the form of inorganic and organic species can be sensitively and unambiguously identified in one single run.

A complete tap water analysis includes the determination of the pH value, the alkalinity and the total water hardness. Both the pH measurement and the pH titration by means of a standard pH electrode suffer from several drawbacks. First, the response time of several minutes is too long and, above all, the stirring rate significantly influences the measured pH value. Unlike these standard pH electrodes, the Aquatrode Plus with its special glass membrane guarantees rapid, correct and very precise pH measurements and pH titrations in solutions that have a low ionic strength or are weakly buffered. Total water hardness is ideally determined by a calcium ion-selective electrode (Ca ISE). In a complexometric titration, calcium and magnesium can be simultaneously determined up to a calcium/magnesium ratio of 10:1. Detection limits for both ions are in the range of 0.01 mmol/L.

A convenient adsorptive cathodic stripping voltammetric (AdCSV) method has been developed for trace determination of uranium(VI) in drinking water samples using chloranilic acid (CAA). The presence of various matrix components (KNO3, Cl-, Cu2+, organics) can impair the determination of the uranium-CAA complex. The interferences can be mitigated, however, by appropriate selection of the voltammetric parameters. While problematic water samples still allow uranium determination in the lower µg/L range, in slightly polluted tap water samples uranium can be determined down to the ng/L range, comparable to the determination by current ICP-MS methods.

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.

This poster looks at the possibility to modify the existing EPA Method to meet California's rigorous public health goal (PHG) of 0.02 µg/L. After optimizing instrument settings and method parameters, a method detection limit (MDL) of 0.01 µg/L is obtained.

Ion chromatography tackles difficult separation problems of various ionic species and typically works with conductivity detection. Mass detection as a secondary independent detector significantly lowers the detection limits and confirms the identity of analytes even when coeluting. This poster describes how the combination of IC-MS and automated sample preparation techniques cope with the analysis of anions and oxoanions in challenging matrices such as soil or explosion residues.

This poster demonstrates the feasibility of coupling a Metrohm IC system to a PerkinElmer NexION ICP-MS, operated under Empower 3 Software.Using a Metrosep Carb 2 column, the chromatographic separation of both species was achieved with a high resolution. Low background and high sensitivity allow determination in the low ng/L range.Optimal separation and full complexation of Cr(III) is already possible with EDTA concentrations from 40 μmol/L in low matrix solutions and may need to be increased depending on the sample matrix.Handling of the system was easy and user friendly. It was shown that speciation of Cr(III) and Cr(VI) can be carried out on this system utilizing a professional data system for acquisition, processing, and reporting.

LC-MS/MS quantification methods are commonly used to determine trace levels of organic compounds. However, highly polar reversed phases (RPs) lack sufficient retention for very polar compounds, or they fail for charged organics. Separation using ion chromatography (IC) and subsequent MS/MS detection is an innovative alternative approach that combines the fast elution and flexibility of the IC system with the excellent resolution and high sensitivity of the MS/MS detector. This poster presents a fast, robust and reliable IC-MS/MS method for the detection of HAAs and other ionic analytes using the high-end MS/MS system QTRAP 6500+ from SCIEX coupled to a the 940 Professional IC Vario One SeS/PP/HPG instrument. This analytical setup is able to identify and quantify the presence of HAAs at trace levels with LLODs between 0.02 μg/mL and 0.2 μg/L on a single HAA. This capability easily fulfills the sensitivity requirements specified in EU Drinking Water Directive, which specifies a maximum residue level (MRL) of 60 mg/mL for the sum of monochloroacetic acid, dichloroacetic acid, trichloroacetic acid, monobromoacetic acid and dibromoacetic acid present in the representative sample.

Lead is known to be highly toxic, and lead salts are easily resorbed by humans. 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. The Lead and Copper Rule (LCR) published by the USEPA (United States Environmental Protection Agency) states an action limit of 15 μg/L lead for drinking water. Using a portable voltammetric instrument, lead can be determined in these concentrations directly at the point of sampling.

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.

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 contains two parts. The first part gives a short theoretical overview while more details are offered in the Metrohm Monograph Conductometry. The second, practice-oriented part deals with the following subjects:Conductivity measurements in general; Determination of the cell constant; Determination of the temperature coefficient; Conductivity measurement in water samples; TDS – Total Dissolved Solids; Conductometric titrations;

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.

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.

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.

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.

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-.

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

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.

Although the known photometric methods for the determination of ammonia/ammonium are accurate, they require a considerable amount of time (Nessler method 30 min, indophenol method 90 min reaction time). A further disadvantage of these methods is that only clear solutions can be measured. Opaque solutions must first be clarified by time-consuming procedures. These problems do not exist with the ion-selective ammonia electrode. Measurements can be easily performed in waste water, liquid fertilizer, and urine as well as in soil extracts. Especially for fresh water and waste water samples several standards, such as ISO 6778, EPA 350.2, EPA 305.3 and ASTM D1426, describe the analysis of ammonium by ion measurement. In this Application Bulletin, the determination according to these standards is described besides the determination of other samples as well as some general tips and tricks on how to handle the ammonia ion selective electrode. Determination of ammonia in ammonium salts, of the nitric acid content in nitrates, and of the nitrogen content of organic compounds with the ion-selective ammonia electrode is based on the principle that the ammonium ion is released as ammonia gas upon addition of excess caustic soda:NH4+ + OH- = NH3 + H2OThe outer membrane of the electrode allows the ammonia to diffuse through. The change in the pH value of the inner electrolyte solution is monitored by a combined glass electrode. If the substance to be measured is not present in the form of an ammonium salt, it must first be converted into one. Organic nitrogen compounds, especially amino compounds are digested according to Kjeldahl by heating with concentrated sulfuric acid. The carbon is oxidized to carbon dioxide in the process while the organic nitrogen is transformed quantitatively into ammonium sulfate.

"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."

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.

This Bulletin, using practical examples, indicates how the user can achieve optimum pH measurements. As this Bulletin is intended for actual practice, the fundamentals - which can be found in numerous books and publications - are treated only briefly.

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 gives a survey of standard methods from the field of water analysis. You will also find the analytical instruments required for the respective determinations and references to the corresponding Metrohm Application Bulletins and Application Notes. The following parameters are dealt with: electrical conductivity, pH value, fluoride, ammonium and Kjeldahl nitrogen, anions and cations by means of ion chromatography, heavy metals by means of voltammetry, chemical oxygen demand (COD), water hardness, free chlorine as well as a few other water constituents.

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 standard method postulated by DIN 38406 Part 16 describes the determination of Zn, Cd, Pb, Cu, Tl, Ni, and Co in drinking, ground, surface and precipitation (e.g. rain) water. Because the presence of organic substances in the water samples can strongly interfere with the voltammetric determination, a pretreatment with UV digestion using hydrogen peroxide is necessary. This digestion ensures the elimination of all organic substances without introduction of blank values. These methods can, of course, also be applied for trace analysis in other materials, e.g. trace analysis in the production of semiconductor chips based on silicon. Zn, Cd, Pb, Cu, and Tl are determined on the HMDE by means of anodic stripping voltammetry (ASV), Ni and Co by means of adsorptive stripping voltammetry (AdSV).

Chlorine is frequently added to drinking water for disinfection. Depending on the reactivity and the concentration of chlorine, toxic disinfection by-products (DBPs) can thereby be released. Therefore, it is necessary to strictly control the chlorine concentration in the drinking water. This Application Bulletin shows how to determine the chlorine concentration according to three standard methods: DIN EN ISO 7939-1, APHA 4500-Cl Method B, and APHA 4500-Cl Method I.

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/LMethod 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.

Copper is one of the few metals which is available in nature also in its metallic form. This and the fact that it is rather easy to smelt led to intense use of this metal already in the so-called Copper and Bronze Age. Nowadays, it is more important than ever, because of its good electrical conductivity and its other physical properties. For plants and animals, it is an essential trace element; for bacteria, in contrast, it is highly toxic.This Application Bulletin describes the determination of copper by anodic stripping voltammetry (ASV) using the scTRACE Gold electrode. With a deposition time of 30 s, the limit of detection is about 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.

Heavy metals, particularly cadmium and lead, are known to be highly toxic to humans. Therefore, controlling the cadmium and lead content in drinking water is of utmost importance. In many countries, the limit in drinking water for cadmium is between 3–5 µg/L, and for lead it is between 5–15 µg/L. These trace concentrations can reliably be determined with the method described in this Application Bulletin. The determination is carried out by anodic stripping voltammetry (ASV) using the non-toxic Bi drop electrode in a slightly acidic electrolyte.

Iron is an essential element in the human diet and is found in many natural and treated waters. Therefore, the World Health Organization (WHO) does not issue a health-based guideline value for iron. Higher concentrations of iron in surface waters can indicate the presence of industrial effluents or outflow from other operations and sources of pollution. Because of this, precise, rapid, and accurate iron determination at low concentrations in environmental and industrial samples is of great importance. This can be achieved with the method described in this Application Bulletin.

Cobalt is an essential element for humans because it is a component of vitamin B12. While small overdoses of cobalt compounds are only slightly toxic to humans, larger doses from 25–30 mg per day may lead to skin, lung, and stomach diseases, as well as liver, heart, and kidney damage, and even cancerous growths. The same is valid for nickel, which can lead to inflammation at higher concentrations. Drinking a large amount of water containing nickel can cause discomfort and nausea. In the EU the legislation specifies 0.02 mg/L as the limit value for the nickel concentration in drinking water. This concentration can be reliably determined with the method described in this Application Bulletin.

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

Partial loop injection is a well known way of sample introduction to HPLC. In ion chromatography, it is not yet used to a large extent. Liquid handling with Metrohm's Dosino technology now enables to use partial loop injection on a highly reproducible and accurate level. It includes multi-level calibration out of one standard solution. This Application Note shows its use for parallel anion and cation determination in tap water applying one single Sample Processor. The anion results are shown in Application Note S–287.

Drinking water analysis is strongly regulated by standards. In this Application Note, the cation determination according to ISO 14911 is shown. The Metrosep C 4 - 150/4.0 is the optimum separation column for this purpose.

The determination of cations in tap water is a simple IC application. Here it is used to present Metrohm's intelligent Pick-up Technique (MiPuT). MiPuT enables the injection of volumes of minimum size from very small sample quantities. In the present case, two volumes of 10 µL from a sample 100 µL in size are used for anion and cation analysis, respectively. The calibration takes place through the injection of various volumes of a single standard solution. AN-S-302 describes the corresponding anion determination.

Reducing the analysis time is a demanding task because it is accompanied by a parallel reduction of peak resolution. With a Microbore column 100 mm in length, standard cations in tap water can be determined in only 5 minutes. Strontium can also be determined by simply extending the run time to 6.5 min.

Fast and handsome IC! Outstanding peak shapes on columns with the standard flow rate and a strong eluent. When the high-capacity Metrosep C 6 - 250/4.0 is used, this usually means long retention times. A strong eluent allows however the determination of the cations in drinking water in a short run time with very symmetrical peaks.

The column stability of the Metrosep C 6 - 250/4.0 was determined in long-term laboratory tests. Two injection series per day were run on each of six days in a row. Each series was comprised of nine tap water injections, three check standard injections and six tap water injections. The IC system was shut down on the seventh day of each series. As a whole, the system ran over 10 weeks and counted a total of 2,150 injections. The results show an outstanding reproducibility and verify the high column stability.

Cation analysis in drinking water is a routine task in ion chromatography and can be achieved with a variety of separating columns. The use of a microbore Metrosep C 6 - 250/2.0 column with a high eluent concentration makes it possible to reduce analysis time to less than 12 minutes. Very symmetrical peaks with high sensitivity for the divalent cations are also achieved. Direct conductivity detection is applied.

Microbore ion chromatography offers better sensitivity, shorter retention times, and consumes less eluent, increasing sample throughput and reducing running costs.

AOF (adsorbable organic fluorine) is used to screen for per- and polyfluorinated alkyl substances in aqueous matrices via pyrohydrolytic combustion and ion chromatography.

Determination of low levels of chloride (to approximately 5 mg/L Cl-) by thermometric titration.

Sulfate is precipitated by reaction with an acidified barium chromate solution. The excess barium chromate is precipitated by basification with ammonia solution. Residual soluble chromate equivalent to the sulfate content of the sample is titrated with a solution of standard ferrous ion to a thermometrically determined endpoint.

Fluoride content in drinking water can be determined quickly and conveniently with the help of potentiometric titration and the ion-selective fluoride electrode (F-ISE). The F-ISE is calibrated with suitable standard solutions before the measurement.

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.

Determination of bromide and bromate in drinking water using anion chromatography with MS detection.

The maximum contaminant concentrations (Maximal Contaminant Level, MCL) of inorganic arsenic and selenium species in drinking water should not exceed 10 and 50 µg/L, respectively. Given that each of the two elements occurs in two oxidation levels – trivalent and pentavalent – a separation step is necessary prior to ICP/MS detection. This Application Note shows the simultaneous determination of the two arsenic (arsenite and arsenate) and selenium species (selenite and selenate). Separation takes place on the Metrosep Dual 3 - 100/4.0 column.

Differentiation between Cr(III) and Cr(VI) is possible following ISO 24384 guidelines by combining ion chromatography with inductively coupled plasma mass spectrometry.

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.

Chlorinating drinking water can form carcinogenic byproducts. EPA Method 557 enables µg/L-level quantification of haloacetic acids using Metrohm IC-MS/MS technology.

During drinking water disinfection with chlorine, chloramine, or ozone, potentially toxic halogenated byproducts can be formed. The disinfectants can react with naturally occurring bromide and/or organic matter in the source water and form one of the most common and highly toxic disinfection byproducts (DBPs): haloacetic acids (HAAs). To protect human health, maximum tolerable levels of HAA in drinking waters are regulated (EPA 816-F-09-004). The EPA Method 557 specifies the analysis of HAAs beside bromate and dalapon by ion chromatography coupled to tandem mass spectroscopy (IC-MS/MS) with LODs varying from 0.02–0.11 µg/L. However, even with single MS, a high sensitivity is achieved to determine the current MCLs within an adequate accuracy. This Application Note describes the analysis of bromate, chlorite, monochloroacetic acid (MCAA), monobromoacetic acid (MBAA), bromochloroacetic acid (BCAA), bromodichloroacetic acid (BDCAA), dibromoacetic acid (DBAA), dichloroacetic acid (DCAA), tribromoacetic acid (TBAA), chlorodibromoacetic acid (CDBAA), and trichloroacetic acid (TCAA) with IC/MS. The Metrohm Driver 2.1 for EmpowerTM offers the analysis as a single software solution with EmpowerTM.

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 silicate in tap water using anion chromatography with direct conductivity detection.

Determination of phenol, m-cresol, 2,6-dimethylphenol and 2,3,6-trimethylphenol in tap water with amperometric detection using a glassy carbon electrode.

Determination of carbonate in tap water using ion-exclusion chromatography with suppressed conductivity detection.

Determination of carbonate in sparkling water using ion-exclusion chromatography with suppressed conductivity detection.

Determination of formate, acetate, propionate, isobutyrate, butyrate, isovalerate, valerate, and capronate added to tap water using anion chromatography with conductivity detection after suppression. The MCS is placed upstream of the chemical suppressor to remove interfering CO2.

The human daily intake of boron from food and beverages is approximately 2 mg. This is far below any toxic level. Some plants, however, are extremely sensitive to boron concentrations above 1 mg/L, e.g., strawberries, blackberries. As seawater contains 4 to 5.5 mg/L of boron, desalination is required to remove surplus boron besides other ions. This application shows the determination of boron (as borate) by ion-exclusion chromatography with conductivity detection after inverse suppression. The method has been optimized to get a sufficient fluoride/borate separation.

Sorbic acid and benzoic acid and their salts are used as food preservatives (E200, E201, E201, E203 and E210, E211, E212, E213 respectively). The content of such preservatives in flavored bottled water may easily be analyzed by ion exclusion chromatography. This method determines the concentration of the respective acid and does not allow differentiating between the counter cations. The determination of sorbic acids and benzoic acid is achieved by conductivity detection after inverse suppression.

Determination of phenol, m-cresol, 2,6-dimethylphenol, and 2,3,6-trimethylphenol in tap water using amperometric detection and a glassy carbon electrode.

The determination of cyanide and sulfide in the trace range requires an alkali eluent and amperometric detection. This Application Note describes a new column/eluent combination for optimized separation. The combination consists of the Metrosep A Supp 10 - 100/2.0 Microbore Column and a sodium hydroxide eluent that contains traces of EDTA for the complexation of the transition metals. This yields a better peak shape and detection limits below 0.05 µg/L.

Drinking water which has been disinfected via the ozonation process can contain undesirable levels of bromate, a carcinogen, via oxidation of bromide in the raw water. Already several agencies including the World Health Organization have recommended concentration limits for bromate set in place to limit its risks to our health. Ion chromatography is mentioned in several analytical standards for the determination of disinfection byproducts (DBP) including bromate, such as EPA 300.1, 317.0, 321.8, 326.0, ASTM D6581, ISO 11206, and ISO 15061. Monitoring trace levels of bromate online means higher throughput and less time spent performing manual laboratory tests, and ensures quality drinking water is produced.

Determination of the anions in potable water using anion chromatography with conductivity detection after chemical suppression.

Determination of chlorite and chlorate in tap water using anion chromatography with conductivity detection after chemical suppression.

Determination of traces of chlorite and bromate in Herisau tap water with direct injection using anion chromatography with conductivity detection after chemical suppression.

Determination of the method detection limit (MDL) and method quantification limit (MQL) of bromate in drinking water using anion chromatography with conductivity detection after chemical suppression.

Determination of bromate in mineral water using anion chromatography with conductivity detection after chemical suppression.

Determination of fluoride, chloride, nitrite, bromide, nitrate, phosphate, sulfate, and iodide in a mineral water 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.

Partial loop injection is a well known way of sample introduction to HPLC. In ion chromatography it is not yet used to a large extent. Liquid handling with Metrohm's Dosino technology now enables to use partial loop injection on a highly reproducible and accurate level. It includes multi-level calibration out of one standard solution. This AN shows its use for parallel anion and cation determination in tap water applying one single Sample Processor. The cation results are shown in Applicatin Note C-133.

VoltIC pro I is the perfect combination of voltammetry and ion chromatography for the fully automated analysis of anions, cations, and heavy metals (e.g., Zn, Cd, Pb, Cu): comprehensive water analysis on a single system.

The determination of anions in tap water is a simple IC application. Here it is used to present Metrohm's intelligent Pick-up Technique (MiPuT). MiPuT enables the injection of volumes of minimum size from very small sample quantities. In the present case, two volumes of 10 µL from a sample 100 µL in size are used for anion and cation analysis, respectively. The calibration takes place through the injection of various volumes of a single standard solution. AN-C-141 describes the corresponding cation determination.

Fast IC means a high sample throughput. This is attained with short columns, relatively high flows and strong eluents. Applied to drinking water analysis this means: determining chloride, nitrate and sulfate within 3 minutes.

Fast IC means short run times and a high sample throughput. This is attained using short columns and strong eluents. Drinking water (including fluoride) is analyzed on the Metrosep A Supp 5 - 100/4.0 under the same conditions as in AN-S-322.

Perchlorate is a wide-spread contaminant in drinking water. Apart from a few natural sources, it usually comes from disinfectants and bleaches as well as rocket fuel. Perchlorate is detected after separation on the Metrosep A Supp 7 - 250/4.0 column using sequential suppression and conductivity detection.

The column stability of the microbore version of the Metrosep A Supp 5 - 250/2.0 was determined in long-term laboratory tests. Two injection series each were run on six days in a row. Each series was comprised of nine tap water injections, three check standard injections and six tap water injections. The IC system was shut down on the seventh day of each series. As a whole, the IC system ran over 12 weeks and counted a total of 2,650 injections. The results show an outstanding reproducibility and verify the high column stability.

The determination of disinfection byproducts is essential for drinking water manufacturers. This Application Note shows the determination of chlorite and bromate in addition to the standard anions. In order to reduce eluent consumption, separation takes place on a Metrosep A Supp 5 - 250/2.0 Microbore column, followed by conductivity detection after sequential suppression.

The stability of the Metrosep A Supp 5 - 250/4.0 column was determined in long-term laboratory tests. Two injection series each were run on six days in a row. Each series was comprised of nine tap water injections, three check standard injections and six tap water injections. The IC system was shut down on the seventh day of each series. As a whole, the IC system ran over 10 weeks and counted a total of 2,150 injections. The results show an outstanding reproducibility and verify the high column stability.

Perchlorate in water is mainly due to anthropogenic sources such as fertilizers, fireworks, rocket fuel, etc. Trace analysis of perchlorate in water samples is a critical task. The high content of standard anions leads to large peaks that interfere with the very small perchlorate peak. In the heart-cut technique, the perchlorate fraction – widely freed of interfering anions – is re-injected onto the column thus providing a sharp peak.

Perchlorate is a wide-spread contaminant in drinking water. In addition to a few natural sources, perchlorate is generally released into drinking water from propellants and from disinfecting and bleaching agents. Convenient separation from other ions is accomplished on a column of the Metrosep A Supp 7 - 250/4.0 type before it is quantified using sequential suppression and conductivity detection. In comparison to AN-S-324, this Application Note shows a considerably lower matrix influence.

VoltIC Professional 1 is the perfect combination of voltammetry and ion chromatography for the fully automated, simultaneous analysis of anions, cations, and heavy metals (e.g., Zn, Cd, Pb, Cu). The multiple-parameter analysis uses the same "Liquid Handling" elements and a shared sample changer, thus saving on space and costs.

Microbore columns with an inner diameter of 2 mm reduce the eluent consumption to about a quarter. Consequently, the detected peak areas of corresponding sample concentration are increased by a factor 4. In this report, the determination of anions in drinking water is described on a Metrosep A Supp 5 - 150/2.0 column.

Ion chromatography (IC) is the method of choice to determine the concentration of common ions in water. This information is crucial as drinking water must meet certain standards to guarantee health (e.g., nitrite and nitrate), as well as technical suitability (e.g., corrosiveness of chloride and sulfate). The Eco IC is an ion chromatograph suitable for economical routine water analysis. Using an A Supp 17 anion column, the analysis of major anions in drinking waters is robust and can be performed at ambient temperatures without additional temperature conditioning.

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.

Perchlorate is known as a potential contaminant in drinking water. Besides very few natural sources, it mainly originates from disinfectants, bleaching, propellants, etc. EPA method 314.0 requires to reach a method detection limit of 0.5 µg/L for perchlorate in reagent water. But also water with a very high content of total dissolved solids needs to be analysed by this method. Making use of the Metrosep A Supp 7 - 250/4.0 column fulfills all requirements of this method.

Determination of disinfection byproducts in water is a standard application for ion chromatography. Applying conductivity detection the separation of chlorite and bromate from chloride is crutial for μg/L detection limits. The combination of a Metrosep A Supp 7 - 250/4.0 and a Metrosep A Supp 16 Guard/4.0 lead to an improved separation. The Limit of Quantification for bromate is around 1 μg/L

The TitrIC flex II system is the perfect combination of titration, direct measurement, and ion chromatography for fully automated analysis of all key parameters. These include pH, conductivity, hardness, anions, cations, as well as the calculation of the ion balance: comprehensive water analysis from one system.

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.

Determination of calcium in aqueous solutions by photometric titration with EDTA using the 610 nm Spectrode.

Determination of citrate in mineral water drinks by potentiometric titration with copper sulfate using the Cu-ISE. Before the determination, the sample is degassed and passed through a cation-exchange resin.

The automated system Basic water analysis determines conductivity, pH value, and alkalinity in all kind of water samples. The high degree of automation (e.g., automated sample addition, automated calibration as well as automated titer and cell constant determination) minimizes errors and guarantees an outstanding reproducibility.

In this application note, a fully automated system is presented which allows the determination of several parameters according to various standards within one analysis. These include conductivity (ISO 7888, EN 27888, ASTM D1125, EPA 120.1), the pH value (EN ISO 10523, ASTM D1293, EPA 150.1), alkalinity (EN ISO 9963, ASTM D1067, EPA 310.1), and Ca/Mg content (ISO 6059, ASTM D1126, EPA 130.2). Additionally, the system transfers the required sample volume into an external titration vessel for the analysis, reducing manual sample preparation. Furthermore, all sensors can be automatically calibrated and the titer of each titrant can also be determined.

In this application note, a fully automated system is presented which allows the determination of several parameters according to various standards within one analysis. These include conductivity (ISO 7888, EN 27888, ASTM D1125, EPA 120.1), pH value (EN ISO 10523, ASTM D1293, EPA 150.1), alkalinity (EN ISO 9963, ASTM D1067, EPA 310.1), and chloride content (ISO 9297, ASTM D512, EPA 325.3). Additionally the system transfers the required volume of sample into an external titration vessel, further reducing manual sample preparation. Furthermore, all sensors can be calibrated automatically and the titer of each titrant can also be determined.

In this application note, a fully automated system is presented which allows the determination of several parameters according to various standards within one analysis. These include conductivity (ISO 7888, EN 27888, ASTM D1125, EPA 120.1), pH value (EN ISO 10523, ASTM D1293, EPA 150.1), alkalinity (EN ISO 9963, ASTM D1067, EPA 310.1), Ca/Mg (ISO 6059, ASTM D1126, EPA 130.2), and chloride (ISO 9297, ASTM D512, EPA 325.3). Additionally the system transfers the required volume of sample into external titration vessels for the different analyses, reducing manual sample preparation. Furthermore, all sensors can be automatically calibrated and the titer of each titrant can also be determined.

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.

The automated system MATi 13 determines the permanganate index in all kind of water samples according to EN ISO 8467. The high degree of automation (e.g., automated sample addition, automated titer and blank value determination) minimizes errors and guarantees robust and reproducible results.

This Application Note describes an automated system with which the chloride content in various water samples can be determined. The high degree of automation (e.g., automated addition of acid and titer determination) reduces errors to a minimum and ensures outstanding reproducibility.

Water hardness is often determined photometrically using two different indicators and while performing the determination at two different pH values. Additionally, the determination itself is subjective, as the color change is determined by the analyst and not by an analytical device.This application note introduces a more robust option to easily assess calcium, magnesium, and total hardness in water by using the Cu-ISE and two different titrants. Sample preparation is identical for both analyses and can therefore be automated without any issues.

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.

The determination of the physical and chemical parameters as electrical conductivity, pH value, alkalinity, the calcium and magnesium hardness as well as the total hardness are necessary for evaluating the water quality. A fast and accurate determination in tap water is realized using an automated OMNIS System working in parallel on different workstations. An 856 Conductivity Module with Dosinos extends the system.

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.

Alkalinity defines the acid-binding capacity of natural water. A distinction is made between total alkalinity (m-value) and carbonate alkalinity (p-value). This Application Note presents the determination of pH and alkalinity in water with a titration method conforming to EPA 310.1, Standard Methods 2320 B (Titration Method), ASTM D1067, EN ISO 9963-1, and EN ISO 9963-2.

Determination of iodate, chlorite, bromate, and nitrite using suppressed anion chromatography with UV/VIS detection after post-column reaction.

Determination of traces of iodide in bottled water using anion chromatography with UV/VIS detection.

Determination of nitrite in mineral water using anion chromatography with UV detection.

Ion chromatography with PCR and UV/VIS detection provides a highly specific and sensitive method for bromate analysis, meeting EPA Method 317 and ISO 11206 requirements.

Chromate (Cr(VI)) or hexavalent chromium is carcinogenic. Its use is restricted. Chromate has to be analyzed in a large range of products starting with drinking water, wastewater (e.g., from leather production), over toys to RoHS-regulated substances. Besides ion chromatographic determination applying conductivity detection, the method described here is suitable especially for lower concentrations.

Hexavalent chromium (chromate) is known to be carcinogenic if inhaled, and suspected to be carcinogenic if ingested. EPA Method 218.7 allows to determine chromate in drinking water down to the sub-µg/L range (method detection limit, MDL = 15 ng/L). Post-column reaction with 1,5-diphenylcarbazide and subsequent visible detection at 530 nm is applied.

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.

Uranium can be determined in drinking water by adsorptive stripping voltammetry (AdSV) at the hanging mercury drop electrode (HMDE). Chloranilic acid is used as complexing agent.

Rhodium and platinum can be determined in water samples after UV digestion and complexation by adsorptive stripping voltammetry (AdSV) at the HMDE.

Cd, Pb, and Cu can be determined in one run in acetate buffer by anodic stripping voltammetry (ASV).

Nickel and cobalt can be determined in drinking water in one run by adsorptive stripping voltammetry (AdSV). Dimethylglyoxime (DMG) is used as complexing agent at a pH value of 9.3.

Manganese in drinking water is determined by anodic stripping voltammetry (ASV) at the HMDE. The measurement is performed in an alkaline solution and zinc solution is added to prevent interference from intermetallic compounds.

The concentration of Fe(III) is determined by adsorptive stripping voltammetry with solochrome violet RS as complexing agent. All reagents have to be added in the order as listed below. Fe(II) does not show any signal. All reagents typically contain iron impurities. Therefore a subtraction of the reagent blank is recommended.

The Se(IV) concentration can be determined by cathodic Stripping Voltammetry (CSV) in an ammonium sulfate electrolyte. The analysis also functions in the presence of Cu. Se(IV) is determined in the first step. In order to register the entire content of Se, Se(VI) species are first reduced to Se(IV). This is handled by the 909 UV Digester at a pH value of between 7 and 9. The method requires practically no reagents and permits selenium speciation.

Aluminum can be determined in drinking water by adsorptive stripping voltammetry at the HMDE using alizarin red S (DASA) as complexing agent. The method is linear up to 35 μg/L. The detection limit for this method is β(Al) = 1 μg/L, the limit of quantification is β(Al) = 3 μg/L. The sensitivity of the method cannot be increased by deposition.

Arsenic is ubiquitous in the earth’s crust in low concentrations. Elevated levels can be found in mineral deposits and ores. Arsenic from such deposits leaches into the groundwater in the form of arsenite (AsO33–) and arsenate (AsO43–), causing its contamination. In addition to the arsenic originating from natural sources, industry and agriculture contribute to the contamination to a lower extent. The guideline value for inorganic total arsenic in the World Health Organization’s «Guidelines for Drinking-water Quality» is set to 10 μg/L. With a limit of detection (LOD) of 0.9 μg/L, anodic stripping voltammetry is a viable, less sophisticated alternative to atomic absorption spectroscopy (AAS) for the determination of arsenic. While AAS (and competing methods) can only be performed in a laboratory, anodic stripping voltammetry can be used conventionally in the laboratory or alternatively in the field using the 946 Portable VA Analyzer. The determination is carried out on the scTRACE Gold electrode.

Arsenic is ubiquitous in the earth’s crust in low concentrations. Elevated levels can be found in mineral deposits and ores. Arsenic from such deposits leaches into the groundwater in the form of arsenite (AsO33–) and arsenate (AsO43–), causing its contamination. As(III) is more toxic than As(V) and shows higher mobility in the environment. The selective determination of this species is possible using the method described in this document.With a limit of detection (LOD) of 0.3 μg/L, anodic stripping voltammetry allows speciation, i.e. the specific determination of As(III). While atomic absorption spectroscopy (AAS) (and competing methods) can only determine the total element concentration, anodic stripping voltammetry is selective to the As(III) oxidation state. The determination is carried out on the scTRACE Gold electrode.

Mercury and its compounds are toxic. The highest risk is posed by chronic poisoning with mercury compounds ingested with food. A significant part of the mercury present in the environment is of anthropogenic origin. Considerable sources are coal-fired power plants, steel, and nonferrous metal production, waste incineration plants, the chemical industry, or artisanal gold mining where the use of elemental mercury for the extraction of gold from the ore is still common. The guideline value for inorganic mercury in the World Health Organization’s «Guidelines for Drinking-water Quality» is set to 6 μg/L.With a limit of detection (LOD) of 0.5 μg/L, anodic stripping voltammetry is a viable, less sophisticated alternative to atomic absorption spectroscopy (AAS).While AAS (and competing methods) can only be performed in a laboratory, anodic stripping voltammetry can be used conventionally in the laboratory or alternatively in the field with the 946 Portable VA Analyzer. The determination is carried out on the scTRACE Gold electrode.

Higher levels of copper in drinking water are usually caused by corrosive action of water leaching copper from copper pipes. While copper is an essential nutrient for the human organism, ingestion of higher concentrations have an adverse effect on human health. The current World Health Organization’s «Guidelines for Drinking-water Quality» recommend a maximum concentration of 2000 μg/L. With a limit of detection (LOD) of 0.5 μg/L, anodic stripping voltammetry is a viable, less sophisticated alternative to atomic absorption spectroscopy (AAS) for the determination of copper in drinking water. While AAS (and competing methods) can only be performed in a laboratory, anodic stripping voltammetry can be used conventionally in the laboratory or alternatively in the field with the 946 Portable VA Analyzer. The determination is carried out on the scTRACE Gold electrode.

Lead is known to be highly toxic to humans as it interferes with enzyme reactions. Chronic lead poisoning can be caused by lead leaching into drinking water from piping systems. The current provisional guideline value in the World Health Organization’s «Guidelines for Drinking-water Quality» sets a maximum concentration of 10 μg/L. With a limit of detection (LOD) of 0.2 μg/L, anodic stripping voltammetry is a viable, less sophisticated alternative to atomic absorption spectroscopy (AAS) to determine lead in drinking water. While AAS (and competing methods) can only be performed in a laboratory, anodic stripping voltammetry can be used conventionally in the laboratory or alternatively in the field with the 946 Portable VA Analyzer. The determination is carried out on a silver film applied to the scTRACE Gold electrode.

Zinc is an essential trace element for humans. Excessive intake of zinc in higher concentrations can be harmful, however. There is no guideline value for zinc in the World Health Organization’s «Guidelines for Drinking-water Quality» because typical levels usually found in drinking water are of no concern. Anodic stripping voltammetry is a viable, less sophisticated alternative to atomic absorption spectroscopy (AAS) for the determination of zinc in drinking water. While AAS (and competing methods) can only be performed in a laboratory, anodic stripping voltammetric determinations can be used conventionally in the laboratory or alternatively in the field using with 946 Portable VA Analyzer. The determination is carried out on the scTRACE Gold electrode.

Iron is an essential element in human nutrition. It can be present in drinking water as a result of water treatment or from corrosion in the water piping system. There is no guideline value for iron in the World Health Organization’s «Guidelines for Drinking-water Quality» because typical levels usually found in drinking water are of no concern. However, there are national limit values in various countries. The European Union has set a guideline indicator value for iron of 200 μg/L. Voltammetry is a viable, less sophisticated alternative to atomic absorption spectroscopy (AAS) for the determination of iron in drinking water. While AAS (and competing methods) can only be performed in a laboratory, anodic stripping voltammetric determinations can be done used conventionally in the laboratory or alternatively in the field using the with 946 Portable VA Analyzer. The determination is carried out with adsorptive stripping voltammetry (AdSV) using 2,3-dihydroxynaphthalene (DHN) on the scTRACE Gold electrode.

Nickel is widely used in stainless steel production. At high enough concentrations, it is known to cause allergic reactions when in contact with skin. Drinking water may be contaminated by taps which are made from metals containing nickel. The guideline value for nickel in the World Health Organization’s «Guidelines for Drinking-water Quality» is set to 70 μg/L. National limit values of typically lower at e. g. 20 μg/L. Cobalt usually occurs associated with nickel and can be found in smaller concentrations besides nickel. Adsorptive stripping voltammetry is a viable, less sophisticated alternative to atomic absorption spectroscopy (AAS) for the determination of nickel and cobalt in drinking water. While AAS (and competing methods) can only be performed in a laboratory, adsorptive stripping voltammetric determinations can be used in the laboratory or alternatively in the field with the 946 Portable VA Analyzer. The determination is carried out on a bismuth film applied to the scTRACE Gold electrode.

Bismuth is considered as a metal with a very low toxicity. In high concentrations toxic effects have been described, however. There is no guideline value for bismuth in the World Health Organization’s «Guidelines for Drinking-water Quality» because typical levels usually found in drinking water are of no concern. Anodic stripping voltammetry is a viable, less sophisticated alternative to atomic absorption spectroscopy (AAS) for the determination of bismuth in drinking water. While AAS (and competing methods) can only be performed in a laboratory, anodic stripping voltammetry can be used in the laboratory or alternatively in the field with the 946 Portable VA Analyzer. The determination is carried out on the scTRACE Gold electrode.

To reduce the toxic effects of cadmium on the human body, as well as to limit the neurotoxic effects of lead, the provisional guideline values in the World Health Organization’s «Guidelines for Drinking-water Quality» are set to a maximum concentration of 3 µg/L for cadmium and 10 µg/L for lead. The completely mercury-free Bi drop electrode takes the next step towards converting voltammetric analysis into a non-toxic approach for heavy metal detection. Using this environmentally friendly sensor for anodic stripping voltammetry (ASV) allows the simultaneous determination of Cd and Pb in drinking water. The outstanding sensitivity is more than sufficient to monitor the provisional WHO guideline values.

The presence of iron in drinking water can lead to an unpleasant taste, stains, or even growth of «iron bacteria» that can clog plumbing and cause an offensive odor. Over a longer period, the formation of insoluble iron deposits is problematic in many industrial and agricultural applications. To avoid these problems, the U.S. Environmental Protection Agency (EPA) defines the Secondary Maximum Contaminant Level (SMCL) for water treatment and processing plants as 0.3 mg/L Fe in drinking water.The voltammetric determination of the iron triethanolamine complex on the non-toxic Bi drop electrode allows both the detection at very low levels (limit of detection of 0.005 mg/L) and measurements in a wide range of concentrations up to 0.5 mg/L.

The main sources of nickel pollution are electroplating, metallurgical operations, or leaching from pipes and fittings. Catalysts for the petroleum and chemical industries are major application fields for cobalt. In both cases, the metal is either released directly, or via the waste water-river pathway into the drinking water system. Therefore in the EU the legislation specifies 20 µg/L as the limit value for the Ni concentration in drinking water.The simultaneous and straightforward determination of nickel and cobalt is based on adsorptive stripping voltammetry (AdSV). The unique properties of the non-toxic Bi drop electrode combined with AdSV results in an excellent performance in terms of sensitivity.

Due to the toxicity and the detrimental effects of nickel and cobalt on human health, their concentrations in drinking water must be controlled. Therefore, EU the legislation specifies 20 µg/L as the limit value for nickel in drinking water. The current provisional guideline value for Ni in the World Health Organization’s «Guidelines for Drinking-water Quality» is set to a maximum concentration of 70 µg/L. To monitor the concentrations of Ni and Co with the 884 Professional VA, a method for simultaneous determination on the glassy carbon electrode (GC-RDE) modified with a Bi film is used.

To reduce the toxic effects of cadmium on the kidneys, skeleton, and the respiratory system, as well as the neurotoxic effects of lead, the provisional guideline values in the World Health Organization’s (WHO) «Guidelines for Drinking-water Quality» are set to a maximum concentration of 3 µg/L for cadmium and 10 µg/L for lead.The powerful anodic stripping voltammetry (ASV) technique on the ex-situ mercury film modified glassy carbon electrode is more than sufficient to monitor the proposed WHO guidelines for Cd and Pb in drinking water.

No health-based guideline value exists for zinc. However, to maintain good quality municipal drinking water, the United States Environmental Protection Agency (US-EPA) set a maximum concentration of 5 mg/L as the limit value. Typical concentrations in surface and ground waters are between 10–40 μg/L Zn, with values up to 1 mg/L in tap water. Anodic stripping voltammetry (ASV) on the ex-situ mercury film modified glassy carbon electrode provides a less complex alternative to atomic absorption spectroscopy (AAS) for zinc determination in drinking water.

The guideline value for chromium in the World Health Organization’s (WHO) «Guidelines for Drinking-water Quality» is 50 µg/L. It should be noted here that chromium concentrations are often expressed as total chromium and not as chromium(III) or (VI). Chromium(VI) is responsible for changes in genetic material, and is found in significantly lower concentrations than Cr(III). Therefore an extremely sensitive method is required to monitor Cr(VI) in drinking water.The powerful adsorptive stripping voltammetry (AdSV) technique on the ex-situ mercury film modified glassy carbon electrode using DTPA as complexing agent can be used to determine such low concentrations.

Presence of thallium in surface water is an indicator of industrial effluents and poses a serious health hazard if imbibed. Monitoring of thallium concentration can easily be done with anodic stripping voltammetry on the silver film modified scTRACE Gold. This non-toxic method allows the determination of thallium concentrations between 10–250 µg/L and can be carried out with the 946 Portable VA Analyzer.

The toxicity of antimony depends on its oxidation state: antimony(III) is more toxic than antimony(V). Due to its carcinogenicity, EU legislation specifies 5 µg/L and the World Health Organization (WHO) sets a maximum concentration of 20 µg/L as the Sb(III) limit value in drinking water.Straightforward determination using anodic stripping voltammetry provides a fast (analysis time under 10 minutes) and an ultra-sensitive tool for monitoring the antimony(III) concentration in drinking water. Measurements can be performed in the laboratory with the 884 Professional VA, or alternatively in the field with the 946 Portable VA Analyzer.

The guideline value for total chromium in the World Health Organization’s (WHO) «Guidelines for Drinking-water Quality» is 50 µg/L. Chromium(VI) is more toxic than its trivalent form (Cr(III)) and is also less abundant. Therefore a robust and sensitive method is required to monitor its concentration in drinking water. The mercury film modified scTRACE Gold can be used to monitor chromium(VI), offering easy handling and a high grade of stability.

The provisional guideline values in the World Health Organization’s (WHO) «Guidelines for Drinking-water Quality» are set to 3 µg/L for cadmium and 10 µg/L for lead. The anodic stripping voltammetry (ASV) technique performed on the ex-situ mercury film modified Metrohm DropSens screen-printed electrode (SPE) can be used to simultaneously detect concentrations as low as 0.3 µg/L for both elements. This is suitable to monitor the WHO guideline values. The main advantage of this method lies in the innovative and cost-effective screen-printed electrode.

EU legislation specifies 20 µg/L as the limit value for nickel in drinking water. The current provisional guideline value for Ni in the World Health Organization’s «Guidelines for Drinking-water Quality» is set to a maximum concentration of 70 µg/L. The adsorptive stripping voltammetry (AdSV) technique performed on the ex-situ bismuth film modified Metrohm DropSens 11L screen-printed electrode (SPE) can be used to simultaneously detect concentrations as low as 0.4 µg/L for nickel and 0.2 µg/L for cobalt with a 30 s deposition time.The disposable, maintenance-free sensor can be used conventionally in the laboratory with the 884 Professional VA, or alternatively in the field with the 946 Portable VA Analyzer. This method is best suited for manual systems.

The difference between the toxic and essential levels of selenium to human health are very slight. Therefore, the current provisional guideline value for selenium(IV) in the World Health Organization’s «Guidelines for Drinking-water Quality» and in the European Drinking Water Directive is set to a maximum concentration of 10 µg/L.The anodic stripping voltammetric (ASV) technique performed on the unmodified scTRACE Gold can be used to determine concentrations as low as 0.5 µg/L selenium with a 30 s deposition time. These limits can be lowered even further by increasing the deposition time. The linear range at 30 s deposition time ends at approximately 100 μg/L. The scTRACE Gold electrode does not need extensive maintenance such as mechanical polishing. Measurements can be performed in the laboratory with the 884 Professional VA or alternatively in the field with the 946 Portable VA Analyzer. This method is suited for manual or automated systems.

Tellurium is one of the elements recently identified as technologically critical for photovoltaic conversion, quantum dots, as well as in thermoelectric technology, and has the potential to become a new emergent contaminant. Until now there is no guideline value in the World Health Organization’s «Guidelines for Drinking-water Quality» and in the European Drinking Water Directive for tellurium(IV) concentration in drinking water.To monitor the tellurium(IV) levels in drinking water, anodic stripping voltammetry (ASV) performed on the unmodified scTRACE Gold is recommended. This method allows determination of tellurium(IV) in the concentration range between 1 µg/L and 60 µg/L when using a 90 s deposition time. The scTRACE Gold electrode does not need extensive maintenance such as mechanical polishing. Measurements can be performed in the laboratory with the 884 Professional VA or alternatively in the field with the 946 Portable VA Analyzer.

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.

This article describes the coupling of ion chromatography with mass spectrometry (IC-MS) and plasma mass spectrometry (IC-ICP/MS) for the trace analysis of potentially hazardous compounds in the environment.

Chromate is allergenic, carcinogenic and extremely toxic. It is therefore subject to strict monitoring. It is present in different concentrations in drinking water, toys, textiles, leather and many other materials. Metrohm has developed various methods for ion chromatographic determination of chromium(VI) which, thanks to Inline Sample Preparation, are suitable for a variety of matrices and concentration ranges – from ng/L to mg/L.

This article describes a simple method for the determination of seven standard anions (fluoride, chloride, nitrite, bromide, nitrate, phosphate and sulfate) in accordance with US EPA Method 300 Part A. An IC system is extended to include Inline Ultrafiltration and Inline Eluent Preparation for the analysis.

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.

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.

High-Performance Liquid Chromatography (HPLC) and Ion Chromatography (IC) are commonly used in the pharma, food, and environmental sectors to analyze samples for specific components and to verify compliance with norms and standards. However, users of HPLC may run into the limitations of this technique, e.g., when analyzing standard anions or certain pharmaceutical impurities. This white paper outlines how such challenges can be overcome with IC.

«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.

Haloacetic acids (HAAs) are commonly produced as disinfection byproducts (DBPs) from water treatment processes. Some HAAs are regulated by the authorities and have been classified as potentially carcinogenic. They have traditionally been analyzed by gas chromatography (GC), a technique that requires time-consuming sample extraction and derivatization, leading to higher costs per analysis. Ion chromatography hyphenated to mass spectrometry (e.g., single or triple quadrupole MS systems) is a powerful tool that can handle many challenging analytical tasks such as measuring μg/L levels of HAAs in potable water samples. This White Paper explains the benefits of using this hyphenated technique for the accurate measurement of HAAs in potable water.

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.

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