Applikationer

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.

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.

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 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).

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.

According to the described method, NTA and EDTA can be determined in mass concentrations of 0.05 mg/L up to 25 mg/L in polluted water and wastewater.At first NTA and EDTA are converted to the corresponding Bi complexes by addition of Bi3+ ions at a pH value of 2.0. As these Bi complexes have significantly different peak potentials, they can be determined simultaneously by DP polarography. The interfering anions nitrite, sulfite, and sulfide are removed from the sample by acidification and purging. Interfering cations are removed by cation exchange; any NTA or EDTA heavy metal complexes present in the sample are disintegrated during this procedure. To remove surfactants and other organic components interfering with the analysis, the sample solution is run through a column filled with non-polar adsorber resin.

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 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."

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

The 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.

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 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).

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 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 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.

Determination of sodium, ammonium, methylamine, guanidine (Gu), and aminoguanidine (Agu) in wastewater using cation chromatography with direct conductivity detection.

Determination of lithium, sodium, ammonium, potassium, manganese, calcium, magnesium, strontium, and barium in an offshore effluent using cation chromatography with direct conductivity detection.

The determination of low ammonium concentrations besides excess sodium is demanding due to the small retention time difference of these two cations. This Application Note shows direct conductivity detection as an ideal means to detect ammonium in a wastewater sample containing 400 mg/L sodium. AN-S-313 shows the analysis of nitrite traces.

Wastewaters often contain high loads of sodium, making the determination of minor cations quite a challenge. In the present wastewater study, the determination of lithium, ammonium, zinc, strontium, and barium is requested. If the sodium concentration exceeds 2 g/L, this negatively influences the peak shape of closely eluting peaks. Applying a appropriate dilution factor to the sample enables the quantification of minor cations. Therefore zinc and barium can be properly quantified with a dilution ratio of 1:2, while lithium and ammonium require minimum dilution factors of at least 1:10 and 1:100, respectively.

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

Cation analysis by IC in wastewater is a proven method. Limiting factor is often the Na/NH4 separation. High sodium concentrations may make ammonium determination impossible due to peak overlapping. The use of sequential suppression and a Dose-in gradient improve the Na/NH4 separation and enables determination of low ammonium concentrations.

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.

Determination of chromium in leather waste solutions in the range between 1000 and 30,000 ppm.

Determination of calcium and magnesium in process solutions.

Determination of sulfide in wastewater by direct potentiometry with the Ag/S ion-selective electrode.

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.

Hexavalent chromium, also referred to as chromate or Cr(VI), is considered toxic and potentially carcinogenic, which is why its concentrations in drinking water should be kept as low as possible. Determination of Cr(VI) is performed by combining ion chromatography with ICP/MS. Separation takes place on the Metrosep A Supp 1 Guard/4.6.

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 fluoride, chloride, nitrite, nitrate, and sulfate in an effluent sample using anion chromatography with direct conductometric detetction.

Determination of perchlorate in process water using anion chromatography with direct conductivity detection.

Determination of iodide in wastewater (dye industry) using anion chromatography with amperometric detection at the silver electrode and dialysis for sample preparation.

Determination of borate in a borate effluent using anion chromatography with direct conductivity detection.

Determination of chloride and sulfate in effluent after Metrohm Inline Dialysis using anion chromatography with direct conductivity detection.

Determination of sulfide in an effluent sample using anion chromatography with amperometric detection.

Determination of boric acid and acetic acid in process water using ion-exclusion chromatography with conductivity detection after chemical suppression.

Sulfide and cyanide are toxic anions. Their trace determination in any kind of water samples, especially in wastewater, is requied for safety reasons. However, metal traces present in the eluent can mask target anions due to complexation. The addition of a stronger complexing agent to the eluent mask these metal cations enabling interference free determaination. This application is mainly used for the analysis of cyanide and/or sulfide in water. However, it also fulfills the requirements of ASTM D2036 for the determination of total, amenable, weak acid dissociable cyanides. The determination of cyanide and sulfide require an alkaline 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 - 100/4.0 column and a sodium hydroxide eluent containing a trace of EDTA for transition metal complexation. This yields in better peak shape and detection limits below 0.1 μg/L.

Ion chromatographic determination of sulfide in wastewater is performed using amperometric detection and an alkali eluent to ensure the stability of the sulfide. Measurements are performed in single-potential or direct current (DC) amperometric mode. It is the best-known and most sensitive amperometric measuring method and also provides, in addition to a high selectivity, a large selection of working electrodes.Sulfide determination is performed on a Metrosep A Supp 10 - 100/4.0 type column; a silver electrode is used as the working electrode.

Cyanide in wastewater is an important parameter to measure for health requirements. Free, weakly complexed, and strongly complexed cyanide can be differentiated. Direct measurement in the wastewater is not feasible due to the matrix itself. Therefore, total cyanide is determined after acidification of the sample, which releases all cyanide from complexes, and subsequent distillation and absorption of cyanide in an alkaline solution. Amperometric detection is applied using a gold working electrode. This electrode is advantageous over the silver electrode due to less contamination issues and better long-term stability.

Gold leaching by cyanidation requires precise monitoring of cyanide and gold. Online process analyzers perform such measurements, improving safety and compliance.

This Process Application Note deals with online measurements of ammonia, nitrite, and nitrate in wastewater treatment plants. These nitrogen compounds are analyzed simultaneously using a drift-free colorimetric measurement in a multi-parameter process analyzer from Metrohm Process Analytics.

Chromium is extracted from chromite ore and is an important part in the production of stainless steel. Chromium is mainly divalent, trivalent and hexavalent in its compounds. In contrast to chromium(III), which is an important trace element and one that is only sparingly soluble in water, hexavalent chromium is extremely toxic and very water-soluble. Cr(VI) is furthermore an important raw material for industry. It must be determined rapidly and precisely in the lower µg/L range in wastewater. Metrohm Applikon offers an array of process analyzers for the analysis of wastewater streams which determine chromium precisely and reproducibly using photometry.

Phosphorus removal is essential in waste water treatment plants to ensure the environmental balance is not upset by discharged effluent. In the treatment facility it is important to know the bioavailable o-phosphate phosphorus (o-PO4-P) concentration in the influent stream either to feed bacteria or to calculate the amount of reagents needed for chemical treatment. For environmental compliance monitoring purposes, treated effluent is monitored for TP – the sum of all insoluble and dissolved phosphates present. With the Metrohm Process Analytics 2035 TP Analyzer (complete with integrated compact digestion cuvette photometer module), you can keep track of both o-PO4-P and TP according to DIN EN ISO 6878:2004-09 around the clock.

Spectroelectrochemistry is a multi-response technique that provides both electrochemical and spectroscopic information about a chemical system in a single experiment, i.e., it offers information from two different points of view. Spectroelectrochemistry focused on the UV/VIS region is one of the most important combinations because this allows us to obtain not only valuable qualitative information, but also outstanding quantitative results. In this application note, the degradation kinetics for 4-nitrophenol, a known pollutant, were determined using SPELEC.

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

Determination of chloride, nitrate, phosphate, and sulfate in wastewater using anion chromatography with conductivity detection after chemical suppression.

Determination of nitrite and nitrate in wastewater using anion chromatography with conductivity detection after chemical suppression.

Determination of sulfate in wastewater after nitric acid combustion using anion chromatography with conductivity detection after chemical suppression.

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 bromide, nitrate, and phosphate in wastewater using anion chromatography with conductivity detection after chemical suppression and dialysis for sample preparation.

Determination of bromide and phosphate in waste dump drainage water in the presence of very high concentrations of other ions and organic substances using anion chromatography with conductivity detection after chemical suppression and dialysis for sample preparation.

Determination of chloride, bromide, and sulfate in photographic process wastewater using anion chromatography with conductivity detection after chemical suppression.

Determination of iodide and thiosulfate in photographic process wastewater using anion chromatography with amperometric detection at the carbon paste electrode after chemical suppression.

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

Determination of chloride, nitrate, bromide, and sulfate in process wastewater using anion chromatography with conductivity detection after chemical suppression.

Determination of fluoride, chloride, nitrate, phosphate, and sulfate in wastewater 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 total phosphate in wastewater after digestion with peroxodisulfate using anion chromatography with conductivity detection after chemical suppression.

Determination of nitrite, nitrate, sulfite, and sulfate in wastewater containing high levels of chloride using anion chromatography with conductivity detection after chemical suppression and after inline chloride removal.

Determination of traces of fluoride, acetate, formate, chloride, and sulfate in an ion exchanger eluate containing 2 g/L nitrate using anion chromatography with a step gradient and conductivity detection after chemical suppression.

Determination of fluoride, acetate, formate, chloride, nitrite, nitrate, phosphate, and sulfate in wastewater containing N-methylpyrrolidone using anion chromatography with conductivity detection after chemical suppression and inline matrix elimination.

Determination of thiooctanoate in wastewater using anion chromatography with conductivity detection after chemical suppression.

Determination of hypophosphite, phosphite, and phosphate in the presence of fluoride, chloride, and sulfate in process water using anion chromatography with suppressed conductivity detection.

Determination of fluoride, acetate, propionate, formate, butyrate, chloride, nitrite, bromide, nitrate, benzoate, phosphate, sulfate, malonate, and oxalate in an industrial process water using anion chromatography with conductivity detection after sequential suppression.

Determination of chloride, nitrate, and sulfate in produced water using anion chromatography with conductivity detection after chemical suppression.

Determination of acetate, chloride, nitrite, bromide, nitrate, phosphate, sulfate, oxalate, fumarate, and molybdate using anion chromatography with conductivity detection after chemical suppression.

The anion column Metrosep A Supp 15 - 150/4.0 is a pretty high-capacity column. The direct determination of arsenate in a matrix of 180 mg/L chloride and 320 mg/L sulfate is not possible, as the arsenate is hardly detectable under the sulfate peak tail. Sample reinjection cuts off the majority of the matrix and therefore allows an accurate determination of the arsenate.

The determination of low nitrite concentrations in the presence of excess sodium chloride is demanding due to the small retention time difference of these two anions. Dual detection – conductivity and UV/VIS – is a powerful method for determining nitrite traces in a 20 g/L sodium matrix. The UV/VIS chromatogram displays no chloride interferences. The determination of ammonium traces in the presence of excess sodium is described in AN-C-145.

Inline Ultrafiltration is a proven sample preparation technique for samples that are slightly or massively contaminated with particles, algae or bacteria. Filtration and injection are coupled and fully automatic. As a rule, 100 or more samples can be filtered through a single membrane. Service life is extended – even with highly contaminated tannery effluent – to more than 300 injections because the filter membrane is rinsed again once more after the analysis with the aid of the Dosino backflush.

Traces of organic acids can be determined only with difficulty in the presence of high concentrations of standard anions, because their small peaks generally disappear under the larger peaks of the standard anions. A simple dose-in-gradient improves the separation: acetate and formate are baseline-separated from fluoride. Furthermore, oxalate elutes considerably less than sulfate. The separation takes place on a column of the Metrosep A Supp 7 - 250/4.0 type with subsequent conductivity detection following sequential suppression.

The Eco IC is an entry-level instrument that is particularly suitable for routine operations and water analysis. It is equipped with a conductivity detector and can be used both with and without chemical suppression. This Application Note describes the determination of anion content with the Metrosep A Supp 17 - 250/4.0 column. This column model is particularly suitable for water analysis at room temperature.

The microbore Metrosep A Supp 4 - 250/2.0 column is particularly suitable for the analysis of anions in critical samples. A waste water sample is being analyzed in the current application. The sample requires only one filtration prior to injection on the Metrosep A Supp 4 - 250/2.0. The anions are quantified with the application of conductivity detection following 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.

Process water from flue gas desulfurization mainly contains sulfite and sulfate. Besides these two main components, other sulfur species may be formed in the process. This application describes the determination of such late-eluting sulfur species with ion chromatography applying a Dose-in gradient. The applied gradient profile enables the resolution of amidosulfonate, dithionate, and imidodisulfonate besides thiosulfate, thiocyanate, major anions, and acetate.

This Application Note presents DPV as a sensitive, selective method for detecting heavy metals in water, detailing setup, parameters, and advantages over other 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.

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.

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.

Nitrogen-based compounds are widely distributed in the environment and are essential growth nutrients for photosynthetic organisms. Therefore, it is important to monitor and control the amount of nitrogen compounds which are released into the environment.In this Application Note, a method to determine the nitrogen content in water by Kjeldahl digestion and distillation followed by a photometric or potentiometric titration according to ASTM D3590 is presented. The universality, precision, and reproducibility of the Kjeldahl method have made it the internationally recognized method for e.g. estimating the protein content in many matrices and it is the standard method to which all other methods are judged against.

Coagulation and flocculation are an essential part of treating both drinking water and wastewater. Aluminum salts such as aluminum sulfate and polyaluminum chloride (PAC) are often used for this purpose. For the precise application and exact dosage of the flocculant, it is important to accurately determine its aluminum content. In this Application Note, the aluminum content is accurately and reliably analyzed based on ABNT NBR 11176 using the 859 Titrotherm equipped with a Thermoprobe HF and sodium fluoride as titrant.

Determination of sulfide and thiosulfate in a process water using anion chromatography with UV/VIS detection after chemical suppression and conductivity detection.

Determination of sulfide in mining wastewater using anion chromatography with UV detection.

Determination of arsenite and arsenate in process water using ion-exclusion chromatography with UV detection.

NTA and EDTA can be determined as their bismuth complexes at the DME.

Zinc, cadmium, lead, and copper can be determined in wastewater samples after UV digestion by anodic stripping voltammetry (ASV) according to DIN 38406 part 16.

Total chromium can be determined in wastewater samples. UV digestion is necessary to remove interfering organic matter before the analysis. Complete oxidation of Cr(III) to Cr(VI) is guaranteed by an additional UV irradiation step at pH > 4.

Mercury can be determined in wastewater by anodic stripping voltammetry (ASV) on a gold rotating disk electrode (Au RDE). After the addition of hydrochloric acid and hydrogen peroxide, digestion is done by UV irradiation.

Determination of nickel and cobalt in wastewater samples through adsorptive Stripping Voltammetry (AdSV). The wastewater samples first undergo a UV digestion in accordance with DIN 38406 Part 16.

Tin can be determined in wastewater by anodic stripping voltammetry (ASV) in oxalate buffer after addition of methylene blue. Samples with organic substances have to undergo UV digestion before analysis. Samples with higher concentrations of metals can be diluted before digestion.

Thallium in wastewater is determined in acetate buffer in presence of EDTA by anodic stripping voltammetry (ASV). Samples with organic substances have to undergo UV digestion before analysis.

Selenium is determined by cathodic stripping voltammetry (CSV) at the hanging mercury drop electrode (HMDE). Se(IV) is deposited on the surface of the mercury drop in sulfuric acid electrolyte under addition of copper ions as Cu xSe y.Wastewater samples containing organic contaminants have to be digested by UV irradiation before analysis. In addition, the sample has to undergo a second irradiation step at pH 7−9 to reduce Se(VI) to Se(IV), since only Se(IV) is electrochemically active.

Cr(VI) is determined by polarography at the SMDE in acetate solution containing ethylene diamine to mask interfering copper ions.Only Cr(VI) is electrochemically active. It is for that reason that all chromium compounds must be present before the analysis as CR(VI), which is guaranteed by UV radiation with a pH > 4.

The concentration of Fe(total) is determined in wastewater after UV digestion. The method is suitable for iron concentrations down to the low μg/L range. Stripping voltammetry is not applicable for this method. Fe(II) and Fe(III) generate signals with identical sensitivity.

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.

This article describes the investigation using ion chromatography and subsequent inductively coupled plasma mass spectronomy (ICP/MS) to determine the extent to which the iron(III) flocculation carried out in the context of wastewater treatment releases toxic gadolinium(III) ions as the result of recomplexing.

On the basis of the experiments that have been performed, it is possible to determine the effectiveness of the ozonization of iodized X-ray contrast media using IC-ICP-MS via the amount of iodate formed. Whereas a 120-minute ozonization guarantees a practically quantitative decomposition of amidotrizoic acid to iodate, approximately 16% of the Iomeprol is still present under the same ozonization conditions. Given that only 14% is present in iodate form in the absence of iodide anions and given that additional, not yet identified peaks occur in the ion chromatogram, the presence of additional decomposition products containing iodine must be assumed. Nonetheless, it is not possible to detect the intact iodized X-ray contrast media with the selected ion chromatographic conditions. Furthermore, the possibility exists of identifying the peak of the unknown decomposition product of the Iomeprol using IC-ESI-TOF-MS.

This Metrohm White Paper presents the important role of electrochemistry in the environmental sciences. The applications have to do with basic research for the fuel cell that yields energy from wastewater, the electrical clean-up of contaminated soil and electrochemical CO2 reduction of greenhouse gases for isolating chemical raw materials.

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.

The analytical challenges of environmental analysis increase in difficulty from year to year. As well as analysis of particularly toxic types of metals such as chromium(VI), highly diverse and partially persistent organic fluorine compounds (e.g., trifluoroacetic acid) are presently in focus. The analysis of toxic oxohalides such as bromate and perchlorate is also a current subject of investigation.

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.

This White Paper gives an overview of the energy-intensive nitrification process that converts ammonia into less harmful nitrogen compounds at wastewater treatment plants (WWTPs). It displays the results from a field test at a WWTP, showcasing the positive influence of single-method process analyzers on the efficiency of the nitrification process.

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