Applications

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.

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 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 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.

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, 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.

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

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

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.

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

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.

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

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

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.

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.

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.

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.

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

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.

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.

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 nitrite and nitrate in wastewater 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 chloride, bromide, and sulfate in photographic process 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 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 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 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.

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.

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.

Determination of sulfate in wastewater after nitric acid combustion using anion chromatography with conductivity detection 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 fluoride, chloride, nitrate, phosphate, and sulfate in wastewater 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.

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.

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

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.

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.

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.

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.

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.