Applications

Determination of acetate, chloride, citrate, and sulfate in a concentrate of an infusion solution using anion chromatography with direct conductivity detection. Non-suppressed IC is used to avoid interferences by the amino acids.

Determination of iodide in a human 24 hour urine sample using anion chromatography with amperometric detection after chemical suppression. The result agrees with that of the photometric method. UV detection did not work.

Determination of the cross contamination of 100 mg/L of fluoride, chloride, nitrite, bromide, nitrate, phosphate, and sulfate to ultrapure water using anion chromatography with conductivity detection after chemical suppression and inline ultrafiltration.

Determination of acetic, propionic, butyric, valeric, and caproic acid in produced water using anion chromatography with conductivity and MS detection after post-column addition of ammonia for MS detection and inline sample preparation by dialysis.

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

Determination of silicate, sulfate, and phosphate in a clay extract using anion chromatography with conductivity detection before and after chemical suppression. Using a step gradient and switching valve to work with or without chemical suppression.

Determination of chloride and sulfate in dust using anion chromatography with conductivity detection after chemical suppression.Sample:dust sampleSample preparation:0.1 g of dust dissolved in 100 mL c(HNO3) = 0.02 mol/L 0.45 µm filtration

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.

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 fluoride, chloride, bromide and sulfate in residual solvent using combustion digestion as sample preparation and subsequent anion chromatography with conductivity detection following sequential suppression. The analysis is significant for use in dividing waste products into non-halogenated and halogenated solvents.Keyword: pyrohydrolysis

Polydextrose is a low-calorie, synthetic polymer made of glucose. It is a recognized additive for foodstuffs. Hot water is used to extract the polydextrose from the foodstuff, after which it is centrifuged. Subsequent fermentation removes maltooligomers and fructans. Afterwards, the polydextrose is quantified using anion-exchange chromatography with pulsed amperometric detection.

The determination of chromium in metal plate samples using anion exchange chromatography with UV/VIS detection after post-column reaction with diphenylcarbazide as per IEC 62321 method for RoHS testing. This method provides procedures for the determination of the presence of chromium(VI) in colorless and colored chromate coatings on metallic samples.

Complexing agents are used in fertilizers to bind trace nutrients such as cobalt, iron, manganese, etc. EN 13368-1 describes the determination of EDTA, HEDTA, and DTPA. As sample preparation, Fe3+ is added to build complexes with the three agents. The complexes are separated on an anion-exchange column and detected by UV/VIS after addition of perchloric acid.

The manufacture of ultrapure water for the pharmaceuticals industry or the semiconductor industry requires high-quality ion exchangers. Metrohm Combustion Ion Chromatography is an indispensable tool in this connection for testing the purity of anion exchange material. The output sample was wet and had to be dried at 105 °C in a special oven with waste air evacuation.Keyword: pyrohydrolysis

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.

Eluent preparation on demand (EPOD) is the convenient and flexible way of automatic eluent preparation. The 849 Level Control together with an 800 Dosino equipped with a 50 mL dosing unit are used to dilute an eluent concentrate to the required eluent concentration. The use of eluent concentrates is suitable for any eluent. This facilitates unattended operation of the system over several weeks (see AN S-296 for anion eluent preparation).

Calibration of fluoride, chloride, nitrite, bromide, nitrate, phosphate, and sulfate using intelligent partial loop injection technique and anion chromatography with conductivity detection after sequential suppression. This technique allows a calibration range of 1:100 (e.g. 1 μg/L to 100 μg/L corresponding to 2 μL to 200 μL injected volume) out of 1 calibration solution. Applying the full range of partial loop injection to the samples one calibration covers a sample concentration range of 1 to 10'000.

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.

Lucigenin is one of the most often used chemiluminescent reagents and might be used for e.g., the indication of the presence of superoxide anion radicals.Lucigenin is rather expensive to buy, however, its synthesis only includes a two stage synthesis starting from acridanone. The first stage includes an Nmethylation, the second forms the lucigenin chloride, which is finally transformed into lucigenin nitrate. To check the purity of the synthesized lucigenin, ion measurement can be applied using a nitrate selective electrode. This is a fast and inexpensive method compared to competing methods such as ion chromatography.

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.

The combination of 850 Professional IC, 858 Professional Sample Processor, Dosino and MagIC NetTM software offers a variety of automated ion chromatographic sample preparation and calibration techniques available as an anion, cation or dual channel system. Calibration is straightforward and requires only one multi-ion standard.Inline calibration allows the calibration of any standard concentration in the ppt range by using one single stable standard solution at the ppb level. By using a preconcentration column and switching the valves one, two or more times different calibration concentrations at the ultra-trace level can be created with unprecedented reproducibility. The inline preconcentration technique uses a pre-concentration column and is ideally suited for trace analysis in complex matrices, especially when combined with matrix elimination. Besides facilitating the preparation of g/L to ng/L calibration graphs Metrohm`s intelligent techniques are capable of logical decision making. While Metrohm`s intelligent Partial Loop technique (MiPT) allows samples with a wide concentration range to be injected without previous manual dilution, the intelligent inline dilution technique, after the first sample injection, compares peak areas, calculates, if necessary, the dilution factor, dilutes and automatically re-injects the sample. The presented inline techniques allow the rationalization of the time-consuming, error-prone and cost-intensive manual preparation of standard solutions. They guarantee that the determined sample concentrations always lie within the calibration range. Higher sample throughputs as well as lower analysis costs and improved data reliability are achieved.

This work was carried out with a Metrosep C 2 - 150 separation column, the following eluent parameters being investigated: nitric, tartaric, citric and oxalic acid concentration and concentration of the complexing anion of dipicolinic acid (DPA). The aim was to determine the effect of these parameters plus that of the column temperature on the retention times of alkali metals, alkaline earth metals, ammonium and amines using ion exchange chromatography with non-suppressed conductivity detection. Due to similar affinities for the ion exchange column, transition metals are difficult to separate with the classical nitric, tartaric, citric and oxalic acid eluents. Partial complexation with the dipicolinate ligand significantly shortens the retention times and improves the separation efficiency. However, too strong complexation results in a rapid passage through the column and thus in a complete loss of separation. Apart from a change in the elution order of magnesium and calcium at high DPA concentrations, other non-amine cations are only slightly affected by the eluent composition. Irrespective of the tartaric acid and nitric acid concentration in the eluent, an increase in column temperature shortens the retention times and slightly improves the peak symmetries of organic amine cations, particularly in the case of the trimethylamine cation. In contrast, an increase in column temperature in the presence of DPA concentrations exceeding 0.02 mmol/L increases the retention time of the transition metals. Depending on the separation problem, variation of the pH value, the use of a complexing agent and/or an increase in column temperature are powerful tools for broadening the scope of cation chromatography.

Anion analysis in milk requires a sophisticated sample preparation to avoid column fouling by fats or proteins. Here Metrohm Inline Dialysis is the perfect automated technique. In dairy products iodide, thiocyanate, and perchlorate need to be determined regularly for health and hygiene reasons. This application allows for the first time to analyze these three components in this matrix within one run.

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

This Application Note documents the suitability of hand-held Raman spectrometers, e.g., the Mira M-1, for the identification and differentiation of salts such as carbonates, phosphates, and sulfates. The focus of the work was the rating of the influence of the cationic part and of the crystal water on the Raman spectroscopy identification of the salts.

Standardization of cetyl pyridinium chloride solutions for use as a cationic surfactant titrant in the determination ofanionic surfactants such as sodium lauryl ether sulfate.

Accurate, reliable determination of ionic surfactants with the Epton two-phase titration method can be achieved using an OMNIS system as shown in this study.

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.

Efficiently analyze food products with ion chromatography (IC). Discover its robust applications in quality control for beverages, food additives, and dairy.

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.

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

The standardization of the cationic surfactant TEGOtrant is performed using potentiometric titration as well as near-infrared spectroscopy (NIRS) in this application.

This Application Note describes carbonate determination with ion chromatography in a 50% sodium hydroxide solution. Sodium hydroxide solutions form carbonates through the absorption of carbon dioxide from ambient air. The carbonate content of an NaOH solution is determined using ion-exclusion chromatography with subsequent conductivity detection following inverse suppression. The samples are diluted 1:20 prior to the analysis and – in order to prevent CO2 absorption – stored in closed sample vessels.

Potassium chloride and potassium bicarbonate effervescent tablets are used to prevent potassium deficiency. Pharmaceutical manufacturers and labs adhere to strict quality regulations using USP-NF monographs. Ion chromatography with suppressed conductivity detection, utilizing the Metrosep A Supp 16 - 100/4.0 (L91) column, is approved by the USP to quantify chloride content in these tablets, following validation per USP General Chapter <621>.

Copper is used widely in industrial cooling water systems for its heat transfer properties, although it is susceptible to corrosion. Corrosion can cause a loss of efficiency and eventually a failure of equipment, leading to costly maintenance, replacement, and downtime. Corrosion inhibitors (triazoles) can be added to the water chemistry, which form sparingly soluble protective layers on the surface of the metal. Triazole concentrations must be maintained to protect the copper, which necessitates regular concentration determinations in cooling water. The 2060 IC Process Analyzer with UV/VIS detection is well-suited for this application, able to precisely and reliably measure multiple ionic and UV-active compounds simultaneously in cooling water.

In severe cases of cyanide poisoning, sodium nitrite is used along with sodium thiosulfate for treatment. This Application Note describes the nitrite ion chromatography assay with the Metrosep A Supp 4 column and suppressed conductivity detection. This column equivalency study was in cooperation with the USP according to the USP General Chapter <621>.

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

Lithium-ion (Li-ion) battery electrolyte quality is essential for performance, stability, and safety reasons. Ion chromatography is an accurate method for electrolyte analysis.

In power plants, corrosion is the primary factor leading to costly and critical downtimes. In a nuclear power plant, a separate water circuit known as the Pressurized Water Reactor (PWR) ensures radioactive material stays contained while still transferring heat and energy to the other circuits. Boric acid and lithium hydroxide are added specially to the PWR circuit in amounts which can complicate other analytical measurements. Lithium prevents corrosion and must be monitored, along with other cations such as zinc, nickel, and ammonium. In order to measure these cations online at sub-µg/L range in a single analysis, the 2060 IC Process Analyzer is offered with combined Inline Preconcentration and Inline Matrix Elimination. Several cations can be analyzed in a single injection, with automated sample preparation making precise and reliable measurements easier.

Application: Free and total carbohydrate determination in instant coffee with IC-PAD according to AOAC 996.04 and ISO 11292.

This Application Note presents an update to the standard AOAC method for total GOS determination in foodstuffs.

This Application Note shows how NIRS is used for the multiparameter analysis of dry matter, pH value, viscosity, and surfactant content in liquid laundry detergent.

An ion chromatography (IC) assay with suppressed conductivity detection is the standardized way to accurately quantify phosphate in phosphates compounded injections.

Anticavity pharmaceuticals like sodium fluoride and acidulated phosphate topical solution products require strict quality control. This Application Note outlines the fluoride IC assay as described in the USP Monograph Sodium Fluoride and Acidulated Phosphate Topical Solution.

Nitrosamine presence in medicines, even at trace level poses high safety risks to patients (carcinogenic). Nitrosamine formation can be avoided by controlling and monitoring the nitrite concentration in pharmaceutical products and substances. This Application Note describes the analysis of nitrite in duloxetine hydrochloride with ion chromatography (IC).

Nitrosamine formation can be avoided by controlling the nitrite concentration in pharmaceutical products and processes. To monitor nitrosamine formation, sensitive analytical methods such as ion chromatography for the determination of nitrite in pharmaceutical products and substances are essential.

Lithium is a soft alkali metal that is typically obtained from salt lake brines. Lithium is used for many applications, but especially for production of lithium-ion batteries in electric cars, mobile phones, and more. This Process Application Note presents a method to monitor lithium as well as other cations in brines by online process ion chromatography (IC), a multiparameter analytical technique that can measure ionic analytes in a wide range of concentrations.

Brilliant Blue (BB) FCF, more commonly known as FD&C Blue #1, is the most commonly used blue dye worldwide for food and beverages. It is generally accepted as safe and non-toxic. Aside from foods labelled as organic or as free from artificial dyes, there is little objection to the use of BB at levels at or exceeding 100 μg/g in foods.This application for Misa (Metrohm Instant SERS Analyzer) is unique. The benefit is twofold — successful detection of a fluorescent dye, and a unique sample cleanup technique that permits detection of a target that does not exhibit a strong SERS signal and is present in a complex matrix. While Misa successfully detects BB in direct sampling, this application describes a simple extraction method that improves detectability of BB with Misa.

Carbon capture systems strip carbon dioxide from flue gases. Online analysis of amines and carbon dioxide enhances amine usage efficiency and reduces operational costs.

Boric acid requires precise monitoring in the primary circuit to control nuclear reactor reactivity. The 2060 TI Process Analyzer monitors boric acid online in near-real time.

This Application Note discusses the standardization of thiosulfate titrant for use in the determination of copper with thermometric titration.

In this Process Application Note, the analysis of low concentrations of calcium and magnesium (0–20 µg/L) in brine is addressed. The presence of calcium and magnesium can shorten the performance and lifetime of the membranes used in the chlor-alkali industry for the production of chlorine. Accurate online monitoring of the hardness is needed in several stages of the process. Other parameters such as acidity, carbonate, hydroxide, silica, alumina, ammonia, iodate and chlorine can also be analyzed online.

In power plants, corrosion is the greatest enemy. If corrosive impurities are present in the circuit streams (e.g., chlorides and hydroxides), deposition of an insulating layer of scale on the heat transfer surfaces occurs, resulting in costly and critical downtimes. To ensure high throughput of power plants, online analysis of critical parameters such as sodium is highly advantageous for safety, protection, and process optimization. With the 2035 Process Analyzer from Metrohm Process Analytics, operators gain the information they need to accurately identify trends, reduce downtimes, and address operational issues before costly problems arise.

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.

Organic halides must be monitored in the environment. Combustion ion chromatography (CIC) is used for accurate halogen analysis in solids following EN 17813:2023.

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

Operando Raman spectroelectrochemistry shows the potential-dependent structural evolution of Ni-based oxygen evolution catalysts, directly linking vibrational signatures to catalytic activity. Correlating these spectroscopic markers with electrochemical performance not only clarifies OER (oxygen evolution reaction) mechanisms but also guides the design of Ni-based catalysts for related oxidation reactions.

The Bayer Process is the method used to refine alumina from bauxite ore, as smelting aluminum directly from alumina is much more cost- and energy-effective. In this process, "aluminate liquors" are created by digesting the crushed bauxite with CaO and NaOH at high temperatures. Additionally, the CaO causticizes carbonate which forms in the alkaline solution from organic degradation and CO2 absorption from the atmosphere. Contaminations are removed at various steps in the process, and the liquor is filtered from the alumina crystals before it is recycled back to the digestion step. Before the spent liquor can be reused, a determination of the concentrations of the total hydroxyl (“caustic”), carbonate, and alumina values is required. These parameters can be determined quickly via thermometric titration with the 2035 Process Analyzer.

Nitrite and nitrate salts are used as preservatives for meat and meat products. Nitrate salts (labeled E 251 or E 252) have a low toxicity but long-term exposure is of concern, as the lower gut reduces them to nitrite, a precursor of nitrosamines (classified as carcinogenic). Nitrite itself is classified as probably carcinogenic to humans. The European Food Safety Authority (EFSA) lists the MPL (maximum permitted levels) after the manufacturing process for nitrite (labeled E 249 or E 250) as between 50–180 mg/kg, and for nitrate between 150–300 mg/kg, depending on the product. The European Commission (Regulation (EC) No 1333/2008) limits nitrate and nitrite salts in processed meat to less than 150 mg/kg. Ion chromatography with UV detection offers a robust and universal method for quality control of nitrite and nitrate in different meat matrices. Additional sample preparation techniques like Inline Ultrafiltration help to save time and costs as well as overcome analysis issues with difficult sample matrices.

Anodizing metal surfaces improves resistance against corrosion and wear. Etching baths can be monitored precisely online with the 2060 TI Process Analyzer or 2026 HD Titrolyzer.

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 EN ISO 18127.

Fenthion is a multi-purpose insecticide used in many countries for mosquito control. To minimize human exposure and the unintentional poisoning of wildlife, the US EPA has classified fenthion as a restricted-use insecticide. However, the widespread spraying of olive orchards in Mediterranean countries results in olive oils that occasionally exceed the maximum residue limits established for olives.Misa (Metrohm Instant SERS Analyzer) easily achieves sensitive trace detection of fenthion in spiked olive oil after a simple organic solvent extraction. This Application Note presents an excellent example of how the signal from SERS substrates can compete with the target signal at very low levels of detection.