Aplikacje

The combination of ion chromatography (IC) and inductively coupled plasma mass spectrometry (ICP/MS) provides a rapid, reliable, and sensitive speciation analysis of wastewater-relevant free and complexed gadolinium compounds. IC-ICP/MS proceeds without costly sample preparation and provides important information on the supply, degradation, and fate of the contrast agents in the (waste)water. The method is also highly suitable for determining compounds containing gadolinium in biological matrixes such as urine or blood.Additionally, IC-ICP/MS is a powerful tool for monitoring inorganic and iodine-containing ionic oxidation byproducts that form during ozonation of iodinated X-contrast media.

In the following tables, the half-wave potentials or peak potentials of 90 metal ions are listed. The half-wave potentials (listed in volts) are measured at the dropping mercury electrode (DME) at 25 °C unless indicated otherwise.

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

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

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

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

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.

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

Determination of sodium, potassium, calcium, and magnesium in the water soluble fraction of a washing powder 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.

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

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

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.

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

Determination of ammonium ions in ammonium salts and mixtures containing ammonium ion.

Determination of chloride in water by direct potentiometry using the Cl-ISE.

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

Cyanides are used in some industrial processes, but if not handled carefully, they could contaminate the wastewater. In an acidic or neutral environment, this contaminated wastewater can form highly toxic hydrogen cyanide gas. Furthermore, the cyanide salts could also poison the environment and enter the ground water system. Therefore, it is essential to monitor the content of cyanide in effluent water. Cyanides can be easily determined with a cyanide ion-selective electrode. This application note presents a method for cyanide analysis according to APHA Method 4500-CN and ASTM D2036.

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

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

Increased fluoride concentrations in water may cause tooth damage, growth disorders, and bone deformation. According to the World Health Organization (WHO), concentrations above 1.5 mg/L are critical.One possible source of fluoride is landfills. Rain washes out harmful substances from landfills which can enter the groundwater. The leachate from landfills should thus be monitored for the fluoride concentration.Ion measurement is a fast and inexpensive method to determine the fluoride content in water samples compared to other methods such as ion chromatography. This Application Note describes a reproducible and accurate measurement of the fluoride content using the fluoride ion-selective electrode with an OMNIS system.

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.

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

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

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.

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.

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.

This Process Application Note details the simultaneous online analysis of H2S and NH3 in sour water which was previously treated in the sour water stripper (SWS). The method includes automatic cleaning and calibration. Fast and accurate results are continuously supplied for process control.

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.

Incineration flue gas requires treatment such as wet scrubbing. The 2060 VA Process Analyzer monitors heavy metals in the scrubbing water, ensuring compliance.

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.